Synthesis & characterization of saccharine derivativesAlexander Decker
This document describes the synthesis and characterization of 15 saccharine derivatives. Saccharine was reacted with various carbonyl-containing compounds, ketones, aldehydes, esters, and diesters or amide compounds to form new open chain compounds. The synthesized compounds were characterized using techniques such as melting point determination, FT-IR, H-NMR, and elemental analysis. FT-IR showed characteristic absorption bands corresponding to functional groups present. H-NMR indicated peaks corresponding to protons of functional groups. Elemental analysis and melting points supported the proposed structures and purity of the compounds.
Synthesis and Characterization O-, M- and Para-Toluyl Thiourea Substituted Pa...IOSR Journals
Abstract: Six new derivatives of carbonyl thiourea comprises of o-,m- and p-toluyl at one end of Nitrogen atom and p-methylpyridine or ethyl pyridine at another one end of Nitrogen atom has been synthesized. The compounds are, 2-methyl-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (I), 3-methyl-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (II) and 4-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (III) for Toluyl-MP while 2-methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (IV), 3- methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (V) and 4- methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (VI) for isomer Toluidal-AEP have been successfully synthesized and characterized by elemental analysis, Infrared Spectroscopy analysis (FT-IR), Nuclear Magnetic Resonance Spectroscopy (NMR) and Ultraviolet-visible (UV-vis). All products shown stretching modes of ν(N-H), ν(C=O), ν(C-N), and ν(C=S) around 3276 cm-1, 1671 cm-1, 1315cm-1 and 1148 cm-1 respectively. All products shown two maximum absorption around 262 nm and 290 nm respectively for carbonyl C=O and thione C=S chromophore. Those both values contributed by n -п* transition. 1H nuclear magnetic resonance spectrum showed presence of aromatic, methyl, methine and amide protons except for product III. All products showed presence of carbon thione in 13C nuclear magnetic resonance except for product III. Ionophor interpretation with acetate anion shows color changes by naked eye for compound (I) and (III).
Combined spectra problem (ir, nmr & mass) format of organic moleculesDr. Krishna Swamy. G
This document outlines experiments for using spectroscopy techniques like UV, IR, NMR, and mass spectrometry to determine the structure of organic compounds. It describes collecting spectroscopic data like IR spectra, 1H NMR spectra, 13C NMR spectra, and mass spectra for several unknown compounds. The data would be analyzed by identifying functional groups and interpreting chemical shifts, multiplicities, fragmentations to deduce molecular formulas and structures. The experiments aim to elucidate organic structures using various spectroscopy methods.
A new road for the synthesis and characterization of new enamino benzodiazepinesAlexander Decker
This document describes the synthesis and characterization of new enamino benzodiazepine derivatives. The synthesis involves two steps: first, N-alkylation of 4-phenyl-1H-1,5-benzodiazepin-2(3H)-one 1 with alkyl bromides to yield compounds 2a-2f. Second, reaction of compounds 2a-2f with N,N-dimethylformamide dimethyl acetal yields compounds 4a-4f. The structures of the products were confirmed using NMR, mass spectroscopy, and X-ray crystallography. This efficient synthetic method provides access to novel enamino benzodiazepine compounds with potential pharmacological activity.
Synthesis, characterization, in vitro cytotoxic and antioxidant activities of...ijperSS
ABSTRACT
A series of novel (Z)-3-(2-(4-(2-oxo-2H-chromen-3-yl) thiazol-2-yl-)hydrazono)indolin-2-one (8a-8d, 9) were synthesized with various substituted indole derivatives. Structures of the newly synthesized compounds were elucidated by FT-IR, 1H-NMR, 13C-NMR and API-ES Mass spectral data. The in vitro cytotoxic activities of the complexes measurement against the human cancer T-lymphocyte cell lines. In vitro evaluation of these title complexes revealed cytotoxicity from 6.8-18µg/mL against CEM, 9.2-21µg/mL against L1210, 10-19µg/mL against Molt4/C8, 8-12µg/mL against HL60 and 8-16µg/mL against BEL7402. Coumarin derivatives 8c and 8d showed that quite significant anticancer activities. The antioxidant activity of the synthesized compounds was evaluated by DPPH scavenging method. Compounds 8c, 8d and 9 showed significant antioxidant activity compared with that of standard drug, ascorbic acid.
Key words: Coumarin, DPPH, Cytotoxic activity.
The document reports on the synthesis and characterization of two new heterometallic complexes containing rhenium tricarbonyl and either iron dicarbonylcyclopentadienyl or bis(diphenylphosphino)ethaneplatinum. Complex I [CpFe(CO)2(μ-TePh)]2Re(CO)3Cl was synthesized by reacting CpFe(CO)2TePh with Re(CO)3(THF)2Cl. X-ray crystallography showed it consists of two iron atoms each linked to rhenium by one phenyltellurolate bridge. Complex II (Dppe)Pt(μ-TePh)2Re(CO)
Triethylamine-catalyzed reactions of malononitrile, carbon disulfide, and various oxiranes produce functionalized 2-(1,3-oxathiolan-2-ylidene)malononitriles in good yields. The reaction occurs under mild conditions in toluene with triethylamine as base. The products contain a polarized carbon-carbon double bond, as shown by 13C NMR spectroscopy. A range of substituted oxiranes participate in the reaction, affording diverse oxathiolane products in high regioselectivity.
This document summarizes the synthesis of new C-2, C-3 substituted heterocyclic derivatives of L-ascorbic acid and their characterization and evaluation of bacterial activity. Specifically, it describes the multi-step synthesis of Schiff bases and 1,3-oxazepine derivatives from L-ascorbic acid, including protection of hydroxyl groups, esterification, hydrazide formation, Schiff base formation with substituted benzaldehydes, and Diels-Alder reaction with phthalic anhydride to form 1,3-oxazepines. The synthesized compounds were characterized using melting point, FTIR, and 1H NMR spectroscopy and tested for antibacterial activity against gram-positive and
Synthesis & characterization of saccharine derivativesAlexander Decker
This document describes the synthesis and characterization of 15 saccharine derivatives. Saccharine was reacted with various carbonyl-containing compounds, ketones, aldehydes, esters, and diesters or amide compounds to form new open chain compounds. The synthesized compounds were characterized using techniques such as melting point determination, FT-IR, H-NMR, and elemental analysis. FT-IR showed characteristic absorption bands corresponding to functional groups present. H-NMR indicated peaks corresponding to protons of functional groups. Elemental analysis and melting points supported the proposed structures and purity of the compounds.
Synthesis and Characterization O-, M- and Para-Toluyl Thiourea Substituted Pa...IOSR Journals
Abstract: Six new derivatives of carbonyl thiourea comprises of o-,m- and p-toluyl at one end of Nitrogen atom and p-methylpyridine or ethyl pyridine at another one end of Nitrogen atom has been synthesized. The compounds are, 2-methyl-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (I), 3-methyl-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (II) and 4-N-[(4-methylpyridine-2-yl) carbamothiol] benzamide (III) for Toluyl-MP while 2-methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (IV), 3- methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (V) and 4- methyl-N-[(2-pyridine-2-yl-ethyl) carbamothiol] benzamide (VI) for isomer Toluidal-AEP have been successfully synthesized and characterized by elemental analysis, Infrared Spectroscopy analysis (FT-IR), Nuclear Magnetic Resonance Spectroscopy (NMR) and Ultraviolet-visible (UV-vis). All products shown stretching modes of ν(N-H), ν(C=O), ν(C-N), and ν(C=S) around 3276 cm-1, 1671 cm-1, 1315cm-1 and 1148 cm-1 respectively. All products shown two maximum absorption around 262 nm and 290 nm respectively for carbonyl C=O and thione C=S chromophore. Those both values contributed by n -п* transition. 1H nuclear magnetic resonance spectrum showed presence of aromatic, methyl, methine and amide protons except for product III. All products showed presence of carbon thione in 13C nuclear magnetic resonance except for product III. Ionophor interpretation with acetate anion shows color changes by naked eye for compound (I) and (III).
Combined spectra problem (ir, nmr & mass) format of organic moleculesDr. Krishna Swamy. G
This document outlines experiments for using spectroscopy techniques like UV, IR, NMR, and mass spectrometry to determine the structure of organic compounds. It describes collecting spectroscopic data like IR spectra, 1H NMR spectra, 13C NMR spectra, and mass spectra for several unknown compounds. The data would be analyzed by identifying functional groups and interpreting chemical shifts, multiplicities, fragmentations to deduce molecular formulas and structures. The experiments aim to elucidate organic structures using various spectroscopy methods.
A new road for the synthesis and characterization of new enamino benzodiazepinesAlexander Decker
This document describes the synthesis and characterization of new enamino benzodiazepine derivatives. The synthesis involves two steps: first, N-alkylation of 4-phenyl-1H-1,5-benzodiazepin-2(3H)-one 1 with alkyl bromides to yield compounds 2a-2f. Second, reaction of compounds 2a-2f with N,N-dimethylformamide dimethyl acetal yields compounds 4a-4f. The structures of the products were confirmed using NMR, mass spectroscopy, and X-ray crystallography. This efficient synthetic method provides access to novel enamino benzodiazepine compounds with potential pharmacological activity.
Synthesis, characterization, in vitro cytotoxic and antioxidant activities of...ijperSS
ABSTRACT
A series of novel (Z)-3-(2-(4-(2-oxo-2H-chromen-3-yl) thiazol-2-yl-)hydrazono)indolin-2-one (8a-8d, 9) were synthesized with various substituted indole derivatives. Structures of the newly synthesized compounds were elucidated by FT-IR, 1H-NMR, 13C-NMR and API-ES Mass spectral data. The in vitro cytotoxic activities of the complexes measurement against the human cancer T-lymphocyte cell lines. In vitro evaluation of these title complexes revealed cytotoxicity from 6.8-18µg/mL against CEM, 9.2-21µg/mL against L1210, 10-19µg/mL against Molt4/C8, 8-12µg/mL against HL60 and 8-16µg/mL against BEL7402. Coumarin derivatives 8c and 8d showed that quite significant anticancer activities. The antioxidant activity of the synthesized compounds was evaluated by DPPH scavenging method. Compounds 8c, 8d and 9 showed significant antioxidant activity compared with that of standard drug, ascorbic acid.
Key words: Coumarin, DPPH, Cytotoxic activity.
The document reports on the synthesis and characterization of two new heterometallic complexes containing rhenium tricarbonyl and either iron dicarbonylcyclopentadienyl or bis(diphenylphosphino)ethaneplatinum. Complex I [CpFe(CO)2(μ-TePh)]2Re(CO)3Cl was synthesized by reacting CpFe(CO)2TePh with Re(CO)3(THF)2Cl. X-ray crystallography showed it consists of two iron atoms each linked to rhenium by one phenyltellurolate bridge. Complex II (Dppe)Pt(μ-TePh)2Re(CO)
Triethylamine-catalyzed reactions of malononitrile, carbon disulfide, and various oxiranes produce functionalized 2-(1,3-oxathiolan-2-ylidene)malononitriles in good yields. The reaction occurs under mild conditions in toluene with triethylamine as base. The products contain a polarized carbon-carbon double bond, as shown by 13C NMR spectroscopy. A range of substituted oxiranes participate in the reaction, affording diverse oxathiolane products in high regioselectivity.
This document summarizes the synthesis of new C-2, C-3 substituted heterocyclic derivatives of L-ascorbic acid and their characterization and evaluation of bacterial activity. Specifically, it describes the multi-step synthesis of Schiff bases and 1,3-oxazepine derivatives from L-ascorbic acid, including protection of hydroxyl groups, esterification, hydrazide formation, Schiff base formation with substituted benzaldehydes, and Diels-Alder reaction with phthalic anhydride to form 1,3-oxazepines. The synthesized compounds were characterized using melting point, FTIR, and 1H NMR spectroscopy and tested for antibacterial activity against gram-positive and
This document summarizes the synthesis and spectral properties of some bis-substituted formazans. It outlines the research methodology used, which involved synthesizing various bis-formazans and investigating their spectral properties using NMR, IR, mass and UV-visible spectroscopy. The results show the elemental analysis and spectral data of the synthesized formazans. Absorption in different solvents is also discussed. It was concluded that the lowest yielding formazan was the o-hydroxy derivative, while the m- and p-hydroxy derivatives had higher yields. Future work involving medical applications of the formazans is proposed.
Aieee 2010 Solved paper by Prabhat GauravSahil Gaurav
The document contains a series of instructions and symbols that are difficult to interpret, followed by sections of text in different languages discussing engineering, medical, law, and other entrance exam topics. Numbers, punctuation symbols, and words are interspersed without clear meaning. The document does not have a clear main topic or idea that can be succinctly summarized.
This document describes a study examining the binding of carbon monoxide (CO) to different substituted iron porphyrins in ionic liquids. CO binding properties were analyzed to potentially reduce CO emissions from automobile exhaust. Various tetraaryliron(II) porphyrins were synthesized and their CO binding affinity was examined in the ionic liquid [bmim][PF6]. The study found that substituents on the porphyrin did not significantly affect CO binding in the ionic liquid, which could enhance CO binding to the iron porphyrin complexes. The goal was to develop a method to reduce CO levels in automobile exhaust using metalloporphyrin catalysts.
A copper-catalyzed synthesis of N-sulfonylamidines is reported via a three-component coupling of sulfonyl azides, terminal alkynes, and trialkylamines. The reaction involves the formation of a ketenimine intermediate through 1,3-dipolar cycloaddition of the sulfonyl azide and copper acetylide, which is then trapped by the trialkylamine to form the N-sulfonylamidine product. The method provides a practical route for synthesizing functionalized N-sulfonylamidines in good yields under mild conditions.
N – methyl thiomethylation and n hydroxymethylation of phthalimideAlexander Decker
This document summarizes a study on the N-methyl thiomethylation and N-hydroxymethylation of phthalimide. Phthalimide was refluxed with DMSO and DMSO-acetic anhydride reagent, yielding two new compounds - N-methyl thiomethyl phthalimide (I) and N-hydroxymethyl phthalimide (II). Spectral data including IR, NMR and mass spectrometry were used to determine the structures of compounds I and II. The reactions and mechanisms for the formation of these compounds from the reactions of phthalimide with DMSO and DMSO-acetic anhydride are discussed.
This document describes the synthesis of novel spirooxindole derivatives via a three-component 1,3-dipolar cycloaddition reaction. Various spirooxindole-spiropiperidinone-pyrrolidine and spirooxindole-spiropiperidinone-pyrrolizine derivatives were synthesized in good yields from isatin, sarcosine or L-proline, and Knoevenagel adducts under optimized reaction conditions. The antimicrobial activities of the synthesized compounds were evaluated, with some compounds exhibiting excellent activity against bacteria and fungi, comparable or superior to standard antimicrobial drugs.
This document describes the synthesis and characterization of palladium(II) and platinum(II) complexes containing 1,1-bis(diphenylphosphino)ferrocene (dppf) and heterocyclic thionate ligands. Single crystal X-ray diffraction studies of two complexes, [Pt(Phozt)2(μ2-dppf)] and [Pd(bzoxt)2(μ2-dppf)], show that the ligands are coordinated in a monodentate fashion through the sulfur atom. The complexes were synthesized by reacting [MCl2(μ2-dppf)] (M = Pd, Pt) with two equivalents of potassium salts of heterocyclic th
This document summarizes a research presentation on ionic liquid catalyzed lignin liquefaction. It discusses using various analytical techniques like TPO-MS, FT-IR, RAMAN and NMR to study the mechanism of lignin conversion into aromatic monomers and dimers. Up to 78% of lignin was converted into low molecular weight soluble products at 120°C for 1 hour using Bronsted acidic ionic liquids as catalysts. The catalyst showed no loss of activity after 5 cycles, indicating its stability under the reaction conditions. The proposed mechanism involves the catalyst promoting cleavage of β-O-4, α-O-4, 4-O-5 and other linkages in lignin to form monomers and dimer units.
Microchimica Acta Volume 75 issue 3-4 1981 [doi 10.1007_bf01196393] G. A. Mil...Sekheta Bros Company
This study presents a kinetic method for determining ultramicro quantities of serotonin, 5-hydroxyindolacetic acid, L-dopa, methyldopa, and carbidopa. The method involves reacting these compounds with molybdenum and hydrogen peroxide in a carbonate buffer to form colored products. Kinetic expressions were derived relating the rate of color formation to concentrations of reactants. Optimal conditions were determined and calibration curves showed the method could determine concentrations of the compounds down to the picogram per milliliter level with good precision. Interference studies found most other substances did not interfere at levels above those of the analytes. This sensitive and simple kinetic method is suitable for analyzing these physiologically important
Bidentate Schiff base ligand 3-(3,4-Dihydroxy-phenyl)-2-[(4-dimethylamino-benzylidene)-amino]-2-methyl-propionic acid was prepared and characterized by spectroscopic techniques studies and elemental analysis. The Cd(II), Ni(II), Cu(II), Co(II), Cr(III),and Fe(III) of mixed-ligand complexes were structural explicate through moler conductance , [FT-IR, UV-Vis & AAS], chloride contents, , and magnetic susceptibility measurements. Octahedral geometries have been suggested for all complexes. The Schiff base and its complexes were tested against various bacterial species, two of {gram(G+) and gram(G-)} were shown weak to good activity against all bacteria.
Microchimica Acta Volume 84 issue 5-6 1984 [doi 10.1007_bf01197162] G. A. Mil...Sekheta Bros Company
This document describes a kinetic method for determining morphine concentration in urine samples. The method involves reacting morphine in the sample with hydrogen peroxide and cobalt(II) ions to form a colored compound. The rate of decomposition of this compound is measured photometrically and is directly proportional to the concentration of morphine over a certain range. The method was found to accurately determine morphine concentrations from 1.5 to 12.3 μg/ml in urine samples. It was also applied to analyze urine samples from individuals suspected of taking morphine or heroin and the results correlated well with an established HPLC method.
1) A kinetic method is proposed for the determination of uranium(VI) based on its catalytic action on the decomposition of hydrogen peroxide in alkaline media.
2) The method was optimized and the kinetic expression was derived. Uranium(VI) can be determined in the concentration range of 0.8 to 6.4 μg/ml using the tangent method.
3) The method is selective and enables determination of uranium(VI) in the presence of high concentrations of various interfering ions. It was applied to determine uranium in phosphoric acid and phosphate ores with results matching another method.
Relations between structure and nicotine-like activity: X-ray crystal structu...Georgi Daskalov
Relations
between
structure
and
nicotine-like
activity:
X-ray
crystal
structure
analysis
of
(-)-cytisine
and
(-
)-lobeline
hydrochloride
and
a
comparison
with
(-
)-nicotine
and
other
nicotine-like
compounds
This document summarizes the synthesis and spectral analysis of a novel benzyl derivative of ciprofloxacin (Cip-D) and its copper(II) and cobalt(II) complexes. Cip-D was synthesized by reacting ciprofloxacin with benzyl chloride in the presence of triethylamine to introduce an amide group. Spectral analysis using 1H NMR, IR, and mass spectroscopy confirmed the structure of Cip-D and indicated bonding between the metal ions and Cip-D in the complexes. Analysis showed shifts in peaks for the complexes, indicating coordination between the metal ions and Cip-D. The Cip-D and its Cu(II) and Co(II)
This study investigates the corrosion inhibition of iron by six mono-azo dye derivatives (MAD_1-6) in 2M HNO3 and 2M NaOH solutions using experimental and computational methods. Gravimetric, thermometric, UV-Vis spectrophotometric, and electrochemical polarization techniques were used to determine inhibition efficiencies experimentally. Density functional theory calculations and molecular dynamics simulations were performed to calculate quantum chemical parameters and binding energies on the Fe(110) surface. Theoretical data agreed well with experimental inhibition efficiencies, with MAD_1 and MAD_6 showing the best inhibition in acidic and alkaline solutions, respectively.
This document describes a novel method for synthesizing highly functionalized 3,4-dihydropyrimidin-2(1H)-ones (DHPMs) through 1,4-addition of nucleophiles onto pyrimidin-2(1H)-ones. Ceric ammonium nitrate (CAN) is used as a catalyst to promote the 1,4-addition reaction of indoles and other nucleophiles with pyrimidin-2(1H)-ones to form novel DHPMs in good yields. A variety of substituted indoles undergo regioselective 1,4-addition to form functionalized 4-indolyl-DHPMs. Pyrrole and sodium boroh
International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.
This summary provides the key details from the document in 3 sentences:
The document reports on a study of chromium-catalyzed ethylene oligomerization using bis(benzimidazolemethyl)amine (BIMA) ligands. It finds that N-alkyl-substituted BIMA ligands produce extremely high catalyst activities (>100,000 g mmol-1 h-1 bar-1) and yield alternating distributions of linear α-olefins. The alternating distributions can be explained by a metallacyclic mechanism in which both single and double ethylene insertions into the metallacycle are possible.
This document describes the synthesis and characterization of a Schiff base ligand and its complexes with various metal ions. The ligand (HL) was prepared in two steps by reacting 3-aminoacetophenone with hydrazine monohydrate to form an intermediate, which was then reacted with salicylaldehyde. The ligand was characterized using various techniques. The metal complexes were prepared by reacting the ligand with metal chlorides in a 1:1 molar ratio. The complexes were characterized using techniques such as elemental analysis, molar conductivity, IR spectroscopy, UV-Vis spectroscopy, and magnetic susceptibility measurements. Based on the data, the complexes were found to have tetrahedral geometry except for the nickel complex which was square planar.
Synthesis and characterization of complexes of schiff base [1, 2 diphenyl -...Alexander Decker
This document describes the synthesis and characterization of a Schiff base ligand and its complexes with various metal ions. The ligand (HL) was prepared in two steps by reacting 3-aminoacetophenone with hydrazine monohydrate to form an intermediate, which was then reacted with salicylaldehyde. The ligand was characterized using various techniques. The metal complexes were prepared by reacting the ligand with metal chlorides in a 1:1 molar ratio. The complexes were characterized using techniques such as elemental analysis, conductivity, IR spectroscopy, UV-Vis spectroscopy, and magnetic susceptibility measurements. Based on the data, the complexes were found to have tetrahedral geometry except for the nickel complex which was square planar.
This document summarizes the synthesis and spectral properties of some bis-substituted formazans. It outlines the research methodology used, which involved synthesizing various bis-formazans and investigating their spectral properties using NMR, IR, mass and UV-visible spectroscopy. The results show the elemental analysis and spectral data of the synthesized formazans. Absorption in different solvents is also discussed. It was concluded that the lowest yielding formazan was the o-hydroxy derivative, while the m- and p-hydroxy derivatives had higher yields. Future work involving medical applications of the formazans is proposed.
Aieee 2010 Solved paper by Prabhat GauravSahil Gaurav
The document contains a series of instructions and symbols that are difficult to interpret, followed by sections of text in different languages discussing engineering, medical, law, and other entrance exam topics. Numbers, punctuation symbols, and words are interspersed without clear meaning. The document does not have a clear main topic or idea that can be succinctly summarized.
This document describes a study examining the binding of carbon monoxide (CO) to different substituted iron porphyrins in ionic liquids. CO binding properties were analyzed to potentially reduce CO emissions from automobile exhaust. Various tetraaryliron(II) porphyrins were synthesized and their CO binding affinity was examined in the ionic liquid [bmim][PF6]. The study found that substituents on the porphyrin did not significantly affect CO binding in the ionic liquid, which could enhance CO binding to the iron porphyrin complexes. The goal was to develop a method to reduce CO levels in automobile exhaust using metalloporphyrin catalysts.
A copper-catalyzed synthesis of N-sulfonylamidines is reported via a three-component coupling of sulfonyl azides, terminal alkynes, and trialkylamines. The reaction involves the formation of a ketenimine intermediate through 1,3-dipolar cycloaddition of the sulfonyl azide and copper acetylide, which is then trapped by the trialkylamine to form the N-sulfonylamidine product. The method provides a practical route for synthesizing functionalized N-sulfonylamidines in good yields under mild conditions.
N – methyl thiomethylation and n hydroxymethylation of phthalimideAlexander Decker
This document summarizes a study on the N-methyl thiomethylation and N-hydroxymethylation of phthalimide. Phthalimide was refluxed with DMSO and DMSO-acetic anhydride reagent, yielding two new compounds - N-methyl thiomethyl phthalimide (I) and N-hydroxymethyl phthalimide (II). Spectral data including IR, NMR and mass spectrometry were used to determine the structures of compounds I and II. The reactions and mechanisms for the formation of these compounds from the reactions of phthalimide with DMSO and DMSO-acetic anhydride are discussed.
This document describes the synthesis of novel spirooxindole derivatives via a three-component 1,3-dipolar cycloaddition reaction. Various spirooxindole-spiropiperidinone-pyrrolidine and spirooxindole-spiropiperidinone-pyrrolizine derivatives were synthesized in good yields from isatin, sarcosine or L-proline, and Knoevenagel adducts under optimized reaction conditions. The antimicrobial activities of the synthesized compounds were evaluated, with some compounds exhibiting excellent activity against bacteria and fungi, comparable or superior to standard antimicrobial drugs.
This document describes the synthesis and characterization of palladium(II) and platinum(II) complexes containing 1,1-bis(diphenylphosphino)ferrocene (dppf) and heterocyclic thionate ligands. Single crystal X-ray diffraction studies of two complexes, [Pt(Phozt)2(μ2-dppf)] and [Pd(bzoxt)2(μ2-dppf)], show that the ligands are coordinated in a monodentate fashion through the sulfur atom. The complexes were synthesized by reacting [MCl2(μ2-dppf)] (M = Pd, Pt) with two equivalents of potassium salts of heterocyclic th
This document summarizes a research presentation on ionic liquid catalyzed lignin liquefaction. It discusses using various analytical techniques like TPO-MS, FT-IR, RAMAN and NMR to study the mechanism of lignin conversion into aromatic monomers and dimers. Up to 78% of lignin was converted into low molecular weight soluble products at 120°C for 1 hour using Bronsted acidic ionic liquids as catalysts. The catalyst showed no loss of activity after 5 cycles, indicating its stability under the reaction conditions. The proposed mechanism involves the catalyst promoting cleavage of β-O-4, α-O-4, 4-O-5 and other linkages in lignin to form monomers and dimer units.
Microchimica Acta Volume 75 issue 3-4 1981 [doi 10.1007_bf01196393] G. A. Mil...Sekheta Bros Company
This study presents a kinetic method for determining ultramicro quantities of serotonin, 5-hydroxyindolacetic acid, L-dopa, methyldopa, and carbidopa. The method involves reacting these compounds with molybdenum and hydrogen peroxide in a carbonate buffer to form colored products. Kinetic expressions were derived relating the rate of color formation to concentrations of reactants. Optimal conditions were determined and calibration curves showed the method could determine concentrations of the compounds down to the picogram per milliliter level with good precision. Interference studies found most other substances did not interfere at levels above those of the analytes. This sensitive and simple kinetic method is suitable for analyzing these physiologically important
Bidentate Schiff base ligand 3-(3,4-Dihydroxy-phenyl)-2-[(4-dimethylamino-benzylidene)-amino]-2-methyl-propionic acid was prepared and characterized by spectroscopic techniques studies and elemental analysis. The Cd(II), Ni(II), Cu(II), Co(II), Cr(III),and Fe(III) of mixed-ligand complexes were structural explicate through moler conductance , [FT-IR, UV-Vis & AAS], chloride contents, , and magnetic susceptibility measurements. Octahedral geometries have been suggested for all complexes. The Schiff base and its complexes were tested against various bacterial species, two of {gram(G+) and gram(G-)} were shown weak to good activity against all bacteria.
Microchimica Acta Volume 84 issue 5-6 1984 [doi 10.1007_bf01197162] G. A. Mil...Sekheta Bros Company
This document describes a kinetic method for determining morphine concentration in urine samples. The method involves reacting morphine in the sample with hydrogen peroxide and cobalt(II) ions to form a colored compound. The rate of decomposition of this compound is measured photometrically and is directly proportional to the concentration of morphine over a certain range. The method was found to accurately determine morphine concentrations from 1.5 to 12.3 μg/ml in urine samples. It was also applied to analyze urine samples from individuals suspected of taking morphine or heroin and the results correlated well with an established HPLC method.
1) A kinetic method is proposed for the determination of uranium(VI) based on its catalytic action on the decomposition of hydrogen peroxide in alkaline media.
2) The method was optimized and the kinetic expression was derived. Uranium(VI) can be determined in the concentration range of 0.8 to 6.4 μg/ml using the tangent method.
3) The method is selective and enables determination of uranium(VI) in the presence of high concentrations of various interfering ions. It was applied to determine uranium in phosphoric acid and phosphate ores with results matching another method.
Relations between structure and nicotine-like activity: X-ray crystal structu...Georgi Daskalov
Relations
between
structure
and
nicotine-like
activity:
X-ray
crystal
structure
analysis
of
(-)-cytisine
and
(-
)-lobeline
hydrochloride
and
a
comparison
with
(-
)-nicotine
and
other
nicotine-like
compounds
This document summarizes the synthesis and spectral analysis of a novel benzyl derivative of ciprofloxacin (Cip-D) and its copper(II) and cobalt(II) complexes. Cip-D was synthesized by reacting ciprofloxacin with benzyl chloride in the presence of triethylamine to introduce an amide group. Spectral analysis using 1H NMR, IR, and mass spectroscopy confirmed the structure of Cip-D and indicated bonding between the metal ions and Cip-D in the complexes. Analysis showed shifts in peaks for the complexes, indicating coordination between the metal ions and Cip-D. The Cip-D and its Cu(II) and Co(II)
This study investigates the corrosion inhibition of iron by six mono-azo dye derivatives (MAD_1-6) in 2M HNO3 and 2M NaOH solutions using experimental and computational methods. Gravimetric, thermometric, UV-Vis spectrophotometric, and electrochemical polarization techniques were used to determine inhibition efficiencies experimentally. Density functional theory calculations and molecular dynamics simulations were performed to calculate quantum chemical parameters and binding energies on the Fe(110) surface. Theoretical data agreed well with experimental inhibition efficiencies, with MAD_1 and MAD_6 showing the best inhibition in acidic and alkaline solutions, respectively.
This document describes a novel method for synthesizing highly functionalized 3,4-dihydropyrimidin-2(1H)-ones (DHPMs) through 1,4-addition of nucleophiles onto pyrimidin-2(1H)-ones. Ceric ammonium nitrate (CAN) is used as a catalyst to promote the 1,4-addition reaction of indoles and other nucleophiles with pyrimidin-2(1H)-ones to form novel DHPMs in good yields. A variety of substituted indoles undergo regioselective 1,4-addition to form functionalized 4-indolyl-DHPMs. Pyrrole and sodium boroh
International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.
This summary provides the key details from the document in 3 sentences:
The document reports on a study of chromium-catalyzed ethylene oligomerization using bis(benzimidazolemethyl)amine (BIMA) ligands. It finds that N-alkyl-substituted BIMA ligands produce extremely high catalyst activities (>100,000 g mmol-1 h-1 bar-1) and yield alternating distributions of linear α-olefins. The alternating distributions can be explained by a metallacyclic mechanism in which both single and double ethylene insertions into the metallacycle are possible.
This document describes the synthesis and characterization of a Schiff base ligand and its complexes with various metal ions. The ligand (HL) was prepared in two steps by reacting 3-aminoacetophenone with hydrazine monohydrate to form an intermediate, which was then reacted with salicylaldehyde. The ligand was characterized using various techniques. The metal complexes were prepared by reacting the ligand with metal chlorides in a 1:1 molar ratio. The complexes were characterized using techniques such as elemental analysis, molar conductivity, IR spectroscopy, UV-Vis spectroscopy, and magnetic susceptibility measurements. Based on the data, the complexes were found to have tetrahedral geometry except for the nickel complex which was square planar.
Synthesis and characterization of complexes of schiff base [1, 2 diphenyl -...Alexander Decker
This document describes the synthesis and characterization of a Schiff base ligand and its complexes with various metal ions. The ligand (HL) was prepared in two steps by reacting 3-aminoacetophenone with hydrazine monohydrate to form an intermediate, which was then reacted with salicylaldehyde. The ligand was characterized using various techniques. The metal complexes were prepared by reacting the ligand with metal chlorides in a 1:1 molar ratio. The complexes were characterized using techniques such as elemental analysis, conductivity, IR spectroscopy, UV-Vis spectroscopy, and magnetic susceptibility measurements. Based on the data, the complexes were found to have tetrahedral geometry except for the nickel complex which was square planar.
An efficient synthesis, characterization and antibacterial activity of novel ...iosrjce
IOSR Journal of Applied Chemistry (IOSR-JAC) is a double blind peer reviewed International Journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
Syntheses and Characterizations of Some New N-alkyl, Isoxazole and Dioxazole ...IJAEMSJORNAL
N-alkyl and cycloadducts derivatives of 5-Chloroisatin were synthesized in good to excellent yields. The method evidences a selective N-alkylation when using 1,2-bis (2-chloroethoxy) ethane as efficient spacer at room temperature on the 5-Chloroisatin moiety. A general method for the 1,3-dipolar cycloaddition of 4-Chlorobenzaldoxime to alkynes provides a useful alternative route to get newisoxazole et dioxazole derivatives.
Synthesis And Antibacterial Activity Of 3-[(3-Phenyl-5-Thioxo-1, 5-Dihydro-4h...inventionjournals
A series of 3-[(3-phenyl-5-thioxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)imino]-1,3-dihydro-2Hindole-2-one derivatives were synthesised through the nucleophilic substitution at carbonyl carbon of Isatin. Structure of synthesized compounds were elucidated by using IR, 1H NMR & 13C NMR spectrometry. Synthesised compounds showed significant antibacterial activity against E.coli (ATCC 35218), S.aureus (ATCC 25323), E.faecalis (Clinical isolate), K. Pneumonia, P. aeruginosa (ATCC 27893) using agar well diffusion method.
A new road for the synthesis and characterization of new enamino benzodiazepinesAlexander Decker
This document describes the synthesis and characterization of new enamino benzodiazepine derivatives. The synthesis involves two steps: first, N-alkylation of 4-phenyl-1H-1,5-benzodiazepin-2(3H)-one 1 with alkyl bromides to yield compounds 2a-2f. Second, reaction of compounds 2a-2f with N,N-dimethylformamide dimethyl acetal yields compounds 4a-4f. The structures of the products were confirmed using NMR, mass spectroscopy, and X-ray crystallography. This efficient synthetic method provides access to novel enamino benzodiazepine compounds with potential pharmacological activity.
This document describes a study that used the organic reagent 4-[N-(5-methyl isoxazol-3-yl)benzene sulfonamide azo]-1- Naphthol to extract cerium(III) ions (Ce3+) from an aqueous solution through solvent extraction. Extraction experiments determined the optimal conditions were a pH of 9, a shaking time of 10 minutes, and a Ce3+ ion concentration of 100 micrograms in the aqueous phase. Organic solvent studies showed chloroform gave the highest distribution ratio values for Ce3+ extraction, though dielectric constant did not linearly correlate with extraction among solvents tested. Stoichiometric studies indicated the extracted ion pair complex had a probable 1:
A series of novel 5-[2-(4-fluorobenzyl)-6-aryl-imidazo[2,1-b][1,3,4]thiadiazol-5-ylmethylene] thiazolidine-2,4-dione derivatives (4a-d) were synthesized. These final compounds (4a-d) were synthesized by Knoevenagel condensation of 2-(4-fluorobenzyl)-6-arylimidazo[2,1-b][1,3,4]thiadiazole-5-carbaldehydes (3a-d) with thiazolidine-2,4-dione. All the newly synthesized compounds were screened for their invivo hypoglycemic and hypolipidemic activity in male Wister rats. The Structures of all the newly synthesized compounds were established by analytical and spectral data.
This document describes the spectroscopic analysis of new dihydropyrimidine derivatives synthesized through a multicomponent reaction. Two new compounds, 5-benzoyl-6-methyl-4-phenyl-3,4-dihydropyrimidin-2(1H)-one (KT-01) and 5-benzoyl-4-(4-chlorophenyl)-6-methyl-3,4-dihydropyrimidin-2(1H)-one (KT-03) were synthesized using a Biginelli reaction involving benzoylacetone, benzaldehyde derivatives, and urea. The structures of KT-01 and KT-03 were confirmed using Fourier transform infrared
Terpenes are natural products made of isoprene units. This document discusses different classes of terpenes including monoterpenes, sesquiterpenes, and triterpenes which are classified based on the number of isoprene units. It also describes the biosynthesis pathways and methods for identification of triterpenes including NMR spectroscopy, thin layer chromatography with various spray reagents, and isolation from plant sources. Four new triterpene compounds isolated from green tea and two new compounds from other plants are characterized based on spectral data and chemical properties.
This document summarizes the synthesis and characterization of ligand diimines and their copper(II) and zinc(II) complexes. Two ligand diimines were synthesized - N,N’-Bis(benzylidène)benzene-1,2-diamine (L1) and N,N’-Bis(4-dimethyaminobenzylidene) propane-1,2-diamine (L2) from reactions of ortho-phenylendiamine and 1,2-diaminopropane with benzaldehyde and 4-dimethylaminobenzaldehyde. The corresponding copper(II) and zinc(II) complexes of formulas (L1
This document describes an experiment to separate a mixture of three organic compounds - cinnamic acid, p-toluidine, and anisole - using acid/base extraction with dichloromethane. The compounds are separated using liquid-liquid extraction with hydrochloric acid and sodium hydroxide to isolate the acidic, basic, and neutral compounds into different layers. 1H NMR spectra are taken during the separation process and of the purified compounds to analyze the effectiveness of the separation technique. Percent yields are also calculated for each separated compound.
Synthesis, Spectroscopic study & Biological Activity Of Some Organotin(Iv) De...IOSR Journals
Some di-and triorganotin(IV) derivatives of (2E)-N-methyl-(2
oxo1,2diphenylethylidne)hydrazinecarbothioamide synthesised by the reactions of the corresponding di and
triorganotin(IV) chlorides with the sodium salt of (2E)-N-methyl-(2-
oxo1,2diphenylethylidne)hydrazinecarbothioamide in different molar ratios. These derivatives have been
characterized by elemental analyses ,molecular weights, conductivity measurements and spectral(IR, 1H, 13C
and 119 Sn NMR) studies.
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...IOSRJAC
Compound (2) was prepared from the reaction of ethyl-2-oxo-2H-coumarin-3-carboxylate (1) with ethylcyanoacetate in ethanol containing a catalytic amount of piperidine as catalyst. Compound (2) is the key intermediate for the synthesis of several series of new compounds such as ((pyrimidine, tetrazine, piperidine, oxazepine)-2H-coumarin-2-one derivatives by reaction with selected reagents such as urea, cyanoacetamide, cyanoacetohydrazide, orthoaminophenol and 5-aminotriazole.
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...IOSRJAC
2-oxo-2H-coumarin-3-carbohydrazide (2) which prepared from the reaction of ethyl-2-oxo-2Hcoumarin-3-carboxylate (1) with hydrazine hydrate in ethanol containing a catalytic amount of piperidine mixture consider a good and available starting intermediate for synthesis of series of functionalized coumarins. So, compound (2) was utilized as a key for the synthesis of some new (pyrazole, triazole)-2H- coumarin-2-one derivatives by the reaction with some selected reagents.
Mononuclear and Polynuclear Copper(I) Complexes with a NewN,N',S-Donor Ligan...mariam1020
The document summarizes the synthesis and characterization of copper complexes using a new N,N',S-donor ligand (L). Three copper complexes were synthesized and characterized by X-ray crystallography: 1) a mixed mono/dinuclear complex, 2) a mononuclear complex with L and PPh3, and 3) a polynuclear complex containing a Cu6 core. NMR and conductivity measurements indicate the polynuclear complex dissociates in solution. DFT calculations confirm the cluster structure is more stable than hypothetical mononuclear species.
The document reports the synthesis and characterization of two rhenium complexes: a dinuclear complex fac-(Re(CO)3Br)2(μ-chret) (1) containing the bridging ligand chret, and a mononuclear complex fac-[Re(CO)3(bzch)Br] (2) containing the chelating ligand bzch. Both complexes were characterized using spectroscopic and analytical techniques. Single crystal X-ray diffraction confirmed the solid state structures. Computational methods provided insight into the experimental spectroscopic data and optimized geometries correlated well with experimental structures.
Synthesis and characterization of some metal complexes of 2- Phenyl-3,4-dihyd...IOSRJAC
2-Phenyl-3,4-dihydro-quinazolin-4-yloxy)-acetic acid (L1) metal complexes with Mn2+ , Co2+, Ni2+ Cu2+ , and Zn2+ ions were studied and the structure of the complexes were elucidated using elemental analyses, infrared (IR), 1H nuclear magnetic resonance (NMR), magnetic moment and thermal analysis measurements. Besides the characterization of complexes by physicochemical technique, Biological activities of the synthesized complexes were examined against some microbial strains for evaluation of antibacterial and antifungal activities.
Study of the Electric Properties of Azo/Hydrazone Tautomeric Mixture of the ...Scientific Review SR
An azo/hydrazone mixture of the phenolic azo dye 4-(9-Anthrylazo)-1-naphthol was obtained in 58%
yield. The product was characterized using spectroscopic techniques such as IR, NMR and ms. The electric
conductivity of the tautomeric mixture was investigated in solid phase at ambient temperature. The electric
measurements revealed that the azo derivative has an electric conductivity equals 0.657 10
7
1
cm
1
and
electric resistivity of 1.521545 10
7
cm which falls within the range of the semiconductors’ electric resistivity that ranges between 10
2 and 109cm.
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1. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
Synthesis & Study of Anesthesia Organic Compounds
Dr . Nagham . Mahmood. Aljamali*
Assist.Prof ,Chem. Dep ., College of Education ., Univ . Kufa.Iraq.
*E-mail: Dr.Nagham_mj@yahoo.com ( to corresponding ).
Abstract :
In the present work , mono & bicyclic compounds [1-8] were synthesized as derivatives of analagisic by
alkalytion of 2-aminothiozoline with carbonyl compounds (succinic acid ., chloro aceticacid .,2,5-hexan-dione .,
3-chloro propoyl chloride ), where as the compounds [9-12] were synthesized by condensation between diketone
compounds with (2-amino benzothiazole ,guanine) . The synthesized compounds structures were characarterized
by several methods :{(C.H.N)-analysis , FT.IR-spectra , 1H.NMR-spectra } & melting points .
Keyword: Anesthesia , pharmaceiutical compounds ., diketone
Introduction :
Asystematic investigation of this class of compounds lead revealed that thiazol containing pharmacoactive
agents play important role in medicinal chemistry and has a long history of application in agrochemicals and
pharmaceiuticals industry as a analgesic and anti-inflammatory drugs are prescribed simultaneously in normal
practice.
The target compounds constitute an essential pharmacophore in many naturally occurring and biologically active
agents.Thiazoles fused with different compounds that are known to contribut as antitumor and antimicrobial(1,2).
The mono & bicyclic compounds are class of compounds well known for along time as anesthetic drugsin
surgery such as diazepine compounds(3-5)which were first introduced for the treatment of anxiety (4-6) .
In this study , the synthesized compounds (thiazolo diazepine , benzoimidazol, thiazolo pyrimidone
,benzothiazolo pyrimidine , guano pyrimidine ) are cyclic compounds in which one or more of nitrogen atoms
which contain five , six & seven membered unsaturated rings of mono or bicyclic compounds (3,5) .
In this work , the cyclic nitrogen compounds were synthesized by cyclocondensation of amino compounds with
carbonyl compounds led to formation of mono & bicyclic compounds [1-12] , which used as analgesic ,
relaxative , hypnotic(7,8)& other uses(9-20) .
Experimental :
- All chemical used were supplied from Fluka & BDH-chemical company .
- All measurements were carried out by :
1- Melting points :electro thermal 9300 , melting point engineering LTD , U.K .
2- FT-IR spectra : fourrier transform infrared shimadzu (8300) (FT-IR) ,KBr-disc was performed .
3- H-NMR spectra & (C.H.N)-analysis .
Synthesis of compounds [1-8] :
A mixture of 2 – amino thiazole (0.02 mole , 2gm) was reacted with one of [(0.02 mole , 2.36g) of succinic acid
.,(0.02 mole , 1.89 g) of chloro acetic acid ., (0.02 mole , 2.54g) of 3 –chloro propoyl chloride ., (0.02 mole ,
2.28 )g of 2,5-hexane-dione )] , respectively ,under reflux for (6hrs) in presence of toluene (100ml) ,the mixture
was cooled ,the precipitate was filtered off to produce (85-90)%of compounds [1,3,5,7],respectively .Drops of
piperidine was heated with one of (0.01 mole , 2g of compounds [1] ., 0.01 mole , 1.58 g of compound[3] & 0.01
mole , 1.08 g of o-phenylene diamine ., 0.01 mole ,1.90 g of compounds [5] ., 0.01 mole , 1.96 g of compound[7]
), respectively , with reflux for (5 hrs) in presence toluene (100ml) , precipitate was filtered off &recrystallized
to give (79-81)% of compound [2,4,6,8] respectively .
Synthesis of compound [9-12] :
A mixture of dibnzoyl methane (0.02 mole ,4.48 g ) was refluxed for (6hrs) with one of (0.02 mole ,3g of 2-
amino benzothiazole ., 0.02 mole , 3.02 g of guanine ) , respectively , in presence of toluene (100 ml ) , the
precipitate was filtered off and recrystallized to produce (86 , 88) % of compounds [9 , 11] respectively .
To prepare compounds [10 , 12] , drops of piperidine was heated with one of (0.01 mole , 3.56 gm of compound
[9] ., 0.01 mole , 3.57 gm of compound [11] ) , respectively with reflux for (5 hrs ) in preseuce of toluene (100
ml ) , the precipitate was filtered off & recrystallized to give (80 , 83)% of compounds [10,12],respectively .
54
2. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
O
OH C
C
O
N C CH3
55
Reaction Scheme :
N
S
NH2
ref. (6hrs)
Toluen
O
C
C
OH
OH
O
N
S
NH CO
ref . (5hrs)
Toluen , pipyr
N
S
N
C O
C
O
[1] [2]
CLCH2COOH
N
S
O NH2
NH CH2 C OH
NH2
ref .(5hrs),
Toluen
N
S
NH CH2
C
NH N
CL
C
O
CL
[3]
[4]
N
S
CL
NH CO
ref . (5hrs)
Toluen
N
S
N
C O
[5]
[6]
CH3
CC
CH3
O
O
S
N
CH3
ref . (5hrs)
Toluen
CH3
N C CH3
S
N
C
[7]
[8]
3. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
O
N
CH2
H
Results & Discussion :
All formated compounds [1-12] have been characterized by their melting points & spectroscopic methods
(FT.IR-spectra , (C.H.N)-analysis , &H-NMR-spectra) :
FT.IR- spectra :
In FT.IR –spectra ,the reaction is followed by appearance carboxyl group
( CO-O- ) absorption band at (2615)cm-1& at (1696)cm-1 due to carbonyl
of amide(6) ( CO-NH ) in compound [1] , which disappear & other bands
appear at (1625,1678)cm-1 due to (C=N azomethine ,( )carbonyl of lactam respectively in compound
[2].
FT.IR–spectra of compound [3] is appear absorption band at (2690)cm-1
due to (-OH) in carboxyl group ( CO-O- ) and (1750)cm-1 due to carbonyl(C=O)of carboxyl group , which
also disappear and other bands are appear at 1625 cm-1 due to ( C=N ) azomethine group and at
(1555, 1470)cm-1 due to (C=N) endocyclic of benzoimidazol in compound [4].
FT . IR – spectra of compound [5] is appear absorption band at (1690)
cm-1 due to(3) carbony of amide(6) ( CO-NH ) and at (760) cm-1 due to (C – Cl ) group , which also disappear
and other bands are appear at (1635) cm-1 due to (C = N) azomethine group and at (1565 , 1480) cm-1due to (C –
N) endo cyclic of pyrimidone in compound [6] .
Compound [7] is appear absorption band at (1630) cm-1 due to (C= N)
56
O
C
N
CH2
C
C
O
ref. (6hrs)
Toluen
N
S
NH2
NH2
N
H N
O
N
H
C
N
S N
C
O ref.(5hrs)
Toluen ,Pipyridine
C
N
S
CH
C
N
[9] [10]
C
N
CH2
C
O
N
N
O
H N N
ref. (5hrs)
Toluen
C
N
C
N
N
O
N
N
H
CH
[11] [12]
4. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
azomethine group and at (1720) cm-1 due to ( CO-) carbonyl of ketone , which disappear and other bands are
appear at (3020) cm-1 is due to (= CH2) and at (1540 , 1430) cm-1 is due to (C – N) end o cyclic of diazepine in
compound [8] .
Compound [9] is appear absorption band at (1640) cm-1 is due to (C = N)
azomethine group(3,6) and at (1725) cm-1 is due to (-CO- ) carbonyl group of ketone , which disappear and other
bands are appear at (1570 ,1490)cm-1 is due to (C – N) end o cyclic of pyrimidine in compound [10] .
Compound [11] is appear absorption band at (1620) cm-1 is due to (C =N)
azomethine , at (1690) cm-1 is due to ( CO-NH ) carbonyl of amide and
at (1728) cm-1 is due to ( CO) carbonyl of ketone , which disappear
and other bands are appear at (1533 , 1433)cm-1 is due to (C – N) endo cyclic of pyrimidine , at (3080)cm-1 is
due to (= CH) in compound [12] .
And other data of functional groups show in the following , table (1) H.NMR – spectra :
H . NMR – spectra of compounds [1-12] showed :
Singlet signal at ʆ 10.36 for protons of carboxyl group (- COOH) and at ʆ 9.8 for proton of amide group (-NH–
CO-) in compound [1] , which disappear as a result of cyclization in compound [2] .
Singlet signal at ʆ 10.9 for proton of carboxyl group (-COOH) in compound [3] , which disappear and other
signals are appear at ʆ 8.6 for proton of amine
(-NH-)(3) and at ʆ 7.1 for protons of phenyl group(-Ph-) ,signals atʆ 2.8 for protons of alkene(CH=CH)in cyclein
compound [4] .
Singlet signal at ʆ 9.9 for proton of amide group (-NH–CO-) in compound [5] , which disappear as a result of
formation of cycle in compound [6] .
Triplet signal at ʆ 3.7 for protons of (CO-CH2-CH2-) in compound [7] , which disappear and other signals appear
at ʆ 2.9 is due to methyl in ( C CH CH2 ) and at ʆ 7.9 is due to proton of thiazol(1) ( CH
57
N
S ) in
compound [8] .Singlet signal at ʆ 4.1 for protons of (-CH2-CO-) in compound [9] , which disappear and other
signals appear at ʆ 3.2 for proton of (
CH C
N
) and at ʆ 7.8 is due to proton of thiazol ( CH
S ) in
compound [10] .
Singlet signal at ʆ 9.7 for proton of amide (- NH–CO -) and at ʆ 4.3 is due to protons of (-CO-CH2-) in compound
[11] , which disappear and othersignal is appear at ʆ3.8 is due to proton of (
CH C
) in compound [12]
(C.H.N)–Analysis :
It was found from compared the calculated data with experimentally data of these compounds , the results were
compactable ,the data of analysis , M.F and melting points are listed in table (2).
Appearance of (H.NMR, FI.IR ,C.H.N )-spectra results are strong evidence to synthesized compounds[1-12].
Acknowledgement:
I would like to express my thanks to ((United Arabic Company )) and ((Zaidan Company of Chemical )) in
Jordan for supplied some materials.And express thank to Mr.Audai in Jordan for providing (C.H.N)-element
analytical ,H.NMR-spectra and Melting points.
Table (1) : FT.IR data (cm-1) of compounds[1-12].
Comp.
No.
Structural formula Name of compounds Functional group in every compounds
(importance group)
[1]
2-(3-propanoic amido)-thiazoline ʊ(-NH-CO-):1696s,
(C=N):1512
ʊ( -OH)of carboxyl:2675 m
(C=O)of carboxyl:1750
ʊ(-NH-)of amide :3276m
OH CO
[2] 1,2-(thiazolino)-5,6-dihydro-diazepine
-4,7-dione
(C=N)azo methine:1625
(-N- C =O):1678
(CH=CH):3000
[3]
2-(amino-acetic)- thiazoline ʊ(-NH-CH2):3300
ʊ(OH)of caboxyl:2673
(C=O)of carboxyl:1755
(CH=CH):3005
N
S
NH CO
N
S
N
C O
C
O
N
S
O
NH CH2 C OH
5. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
[4] 2-(2-benzoimidazoline methylene-amino)–
58
thiazoline
ʊ(C=N) azo methine:1625
ʊ(-NH)endo imidazol cycle :3310
(C-N)endo cycle :1555, 1470
(-NH-):3340 ,3310
[5]
2-(2-chloro ethylene amido) –
thiazoline
(O=C-NH-) :1690
(C-Cl):760 ,(-N=C-):1495
(CH=CH):2998
[6]
3,4-tetrahydro thiazolo pyrimidine (C=N):1635
(O=C–N-):1695
(C-N)endo cycle :1565, 1480
(CH=CH):3000
(CH2):2910
[7]
2-(2-hexanone–thiazolidine ). (C=N):1630
(O=C–CH3)ketone :1720
[8]
4,7-dimethyl-1,2- thiazole
diazepine
(C=N):1625 ,
(=CH2):3020
(C-N) endocyclic :1540,1432
N
S
NH CH2 C
N
NH
N
S
CL
NH CO
N
S
N
C O
C
O
CH3
N C CH3
S
N
C
CH3
N C CH3
S
N
[9] 2-(phenyl acetophenone) –
benzothiazolidine.
(C=N)azomethine:1640 ,
( C=O )Ketone :1725
(-C=N)cyclic:1498
(C-S-C):780
[10]
4,6-(diphenyl)-1,2- (benzothiazole)-
pyrimidine
(C=N) azomethine:1635
(C-N) endocycle : 1570 ,1490
(C=C)Alkene:3010
(C=C)Aromatic:1570
C
N
CH2
S N
C
O
C
N
S
CH
C
N
[11] 2-(phenylacetophenon)
guaninopyrimidine
(C=N):1620s
( C=O ) Ketone: 1728s ,
(-NH) endocycle of guanine :3335 br
(CO-NH)Carbonyl of amide in guanine cycle
:1690
C
N
CH2
C
O
N
H
N
O
H N N
[12] 4,6-(diphenyl)-1,2-
guaninopyrimidine
(C=N):1640S ,
(C-N)endocycle : 1533,1433s (C=N)endocyclic
of guanine:1569 s
(O=C-N) carbonyl of amide in guanine cycle
:1695m
(CH=C) alkene :3080
(C=C)Aromatic:1575
C
N
C
CH
N
N
O
N
N
H
S=strong , M= medium , V=very , br=broad
6. Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.6 No.8, 2014
Table (2) :phesical properties and Elemental Analysis of compounds[1-12]
Comp. No. M.F m.p (c°) Calc ∕Found C% H% N%
[1] C7H8N2O3S 160 42.0
41.871
59
4
3.905
14
13.836
[2] C7H6N2O2S 152 46.153
46.026
3.296
3.119
15.384
15.209
[3] C5H6N2O2S 148 37.974
37.785
3.797
3.628
17.721
17.584
[4] C11H10N4S 154 57.391
57.247
4.347
4.214
24.347
24.205
[5] C6H7N2 OSCl 145 37.795
37.603
3.674
3.485
14.698
14.456
[6] C6H6N2OS 136 46.753
46.514
3.896
3.718
18.181
18.049
[7] C9H12N2OS 158 55.102
54.95
6.122
6.037
14.285
14.148
[8] C9H12N2 S 153 60.0
59.81
6.666
6.478
15.555
15.374
[9] C22H16N2OS 174 74.157
74.029
4.494
4.316
7.865
7.657
[10] C22H16N2S 179 77.647
77.459
4.705
4.518
8.235
8.087
[11] C20H15N5O2 184 67.226
67.098
4.201
4.079
19.607 19.405
[12] C20H13N5O 189 70.796
70.558
3.834
3.607
20.648
20.406
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