This document describes the synthesis and characterization of a new cationic surfactant derived from 5-Chloro-1H-indole-2,3-dione. The surfactant was synthesized in two steps: first, 5-Chloroisatin was alkylated with 1,6-dibromohexane under phase transfer catalysis conditions. Second, the product was quaternized with trimethylamine in acetone solution. The structures were confirmed using NMR spectroscopy. The critical micelle concentration of the surfactant in water was determined to be 5.10-3 M using conductivity measurements at room temperature. In conclusion, a new cationic surfactant was successfully synthesized and its micell
Some physicochemical properties such as density, refractive index, solubility, conductance, dissociation constant etc. have been studied for some newly synthesized chalcones in different solvents at 308.15 K.
Ninhydrin Based Visible Spectrophotometric Determination of GemigliptinRatnakaram Venkata Nadh
A simple method is described to determine the amount of gemigliptin in bulk and tablet formulation by visible spectrophotometry. Basis of the proposed method is the reaction of the primary amine present on gemigliptin with ninhydrin in alkaline pH (alkaline borate buffer) medium to produce a purple color (Ruhemann’s purple) which has maximum absorption at 558 nm. The method was validated as per the current ICH guidelines. The obtained regression equation (y = 0.0148x+0.0011) in the range of 5-30 μg mL-1 has a good correlation coefficient (> 0.999). As the method does not require any separation, it is rapid and simple. The recovery levels of the drug were in the range of 99.73 – 99.96. This method is a green method as it no organic solvents were employed
Gelatin-grafted N- proflavine acryl amide was synthesized through two steps; firstly the Gelatin was grafted with
acrylic acid free radically using Ammonium per-sulfate at 60℃, Then it was modified to its corresponding acyl
chloride derivation, second step included the substitution with amino group of proflavine, in this research Gelatin
was used as a natural nontoxic, water soluble polymer as a drug carrier.
The prepared pro drug polymer was characterized by FTIR and 1H-NMR spectroscopies, Controlled drug release
was studied in different pH values at 37℃. Many advantages were obtained comparing with other known
methods.
Mixed Ligand, Palladium(II) and Platinum(II) Complexes of Tertiary Diphosphin...Karwan Omer
Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary
diphosphinesdppm. dppp and dppf with Thioester ligand S-1H benzo[d] imidazole-2-yl benzothioate
(HSBIBT) have been prepared by the reaction of PdCl2 and PtCl2 with one equiv of tertiary
diphosphines ligands to form [Pd(k2-dppf)Cl2], [Pd(k2-dppp)Cl2] and [Pt(k2-dppmCl)Cl2] complexes
and then add the ligand HSBIBT to these complexes to form mixed ligand complexes. The prepared
complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, magnetic
susceptibility, molar conductance, IR spectral data and UV-Visible. The results suggested that the
ligand HSBIBT bonded to the metal through N atom and square planner geometries were assigned
for the complexes.
Synthesis and Pharmacological Evaluation of Novel Heterocyclic CompoundIJSRD
2-[(4-bromo anilino)]-4-chloro-6-morpholino-1,3,5-triazine[2a] and 4-chloro-N-(4-fluorophenyl)-6-morpholino-1,3,5-triazin-2-amine [2b]were synthesized and studied for their biological activity. These compounds were prepared by the condensation of 4-bromoaniline and 4-fluoroaniline with 4-(4,6-dichloro-1,3,5-triazin-2-yl) morpholine [1] which is prepared by the reaction between 2,4,6-trichloro-1,3,5-triazine and morpholine. All the compounds were characterized by elemental analysis and spectral studies.
In this work a new prodrug polymer was
prepared with two attachment groups (amid-ester), using di
functional spacer such as ethanol amine, which could react with
polyacrylic acid producing amide group, with remain ethanol
terminal group which could react with captopril acyl chloride,
producing ester group with extended the arm substituted drug to
improve the hydrolysis and to prevent the steric effect of polymer
chains. Many advantages enhanced the prodrug of polymer. The
prepared polymers were characterized by FTIR, 1H –NMR
spectroscopies. Controlled drug release was studied in different
pH values at 37℃, using UV. Spectra with comparing with
calibration curve. The modification percentage test was studied,and swelling percentage was calculated and all physical properties were observed.
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...IOSRJAC
This research includes synthesis of new heterocyclic derivatives of quinazolinone and studying the possibility for their application as surfactants. The preparation process started by the reaction of pentadecanoyl chloride with anthranilic acid gave 2-pentadecyl-4H-benzo[3,1]oxazin-4-one [1] which was used as starting material to synthesis some heterocyclic compounds by a reaction with nitrogen nucleophiles. Compound [1] as starting material reacted by three ways. The first way react Compound [1] with semicarbazide, thiosemicarbazide and phenylsemicarbazide in pyridine as solvent to obtained [1-(4-oxo-2- pentadecylquinazolin-3(4H)-yl) urea [2], thiourea [3], phenylthiourea [4] respectively]. The second way include the reaction of Compound [1] with 99% hydrazine hydrate to produce 3-amino-2-pentadecylquinazolin- 4(3H)-one [5], then converted to amino derivatives [6-8] by the reaction of Compound [5] with different halogenated compounds such as (benzoyl chloride, acetyl chloride and chloro acetyl chloride ) in DMF and pyridine as catalyst. The third way include the reaction of compound [1] with different substituted amine and amide compounds (thiourea, hydroxylamine hydrochloride, glycine, ammonium acetate and phenyl hydrazine) respectively to obtain derivatives of quinazoline [9-14]. The produced compounds [2,4,5,7 and 12] react with propylene oxide in different moles (n=3, 5 and7) to yield novel groups of nonionic compounds having a function as surface active agents. The surface active properties like surface tension and interfacial tension, wetting time, cloud point, emulsion stability, foam height and CMC of these compounds were measured and showed a pronounced surface activity, good emulsifying properties and highly foaming in some of these compounds. Newly synthesized compounds were identified via spectral methods; their [FTIR and some of them by 1HNMR, 13C-NMR] and measurements of some of its physical properties.
Some physicochemical properties such as density, refractive index, solubility, conductance, dissociation constant etc. have been studied for some newly synthesized chalcones in different solvents at 308.15 K.
Ninhydrin Based Visible Spectrophotometric Determination of GemigliptinRatnakaram Venkata Nadh
A simple method is described to determine the amount of gemigliptin in bulk and tablet formulation by visible spectrophotometry. Basis of the proposed method is the reaction of the primary amine present on gemigliptin with ninhydrin in alkaline pH (alkaline borate buffer) medium to produce a purple color (Ruhemann’s purple) which has maximum absorption at 558 nm. The method was validated as per the current ICH guidelines. The obtained regression equation (y = 0.0148x+0.0011) in the range of 5-30 μg mL-1 has a good correlation coefficient (> 0.999). As the method does not require any separation, it is rapid and simple. The recovery levels of the drug were in the range of 99.73 – 99.96. This method is a green method as it no organic solvents were employed
Gelatin-grafted N- proflavine acryl amide was synthesized through two steps; firstly the Gelatin was grafted with
acrylic acid free radically using Ammonium per-sulfate at 60℃, Then it was modified to its corresponding acyl
chloride derivation, second step included the substitution with amino group of proflavine, in this research Gelatin
was used as a natural nontoxic, water soluble polymer as a drug carrier.
The prepared pro drug polymer was characterized by FTIR and 1H-NMR spectroscopies, Controlled drug release
was studied in different pH values at 37℃. Many advantages were obtained comparing with other known
methods.
Mixed Ligand, Palladium(II) and Platinum(II) Complexes of Tertiary Diphosphin...Karwan Omer
Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary
diphosphinesdppm. dppp and dppf with Thioester ligand S-1H benzo[d] imidazole-2-yl benzothioate
(HSBIBT) have been prepared by the reaction of PdCl2 and PtCl2 with one equiv of tertiary
diphosphines ligands to form [Pd(k2-dppf)Cl2], [Pd(k2-dppp)Cl2] and [Pt(k2-dppmCl)Cl2] complexes
and then add the ligand HSBIBT to these complexes to form mixed ligand complexes. The prepared
complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, magnetic
susceptibility, molar conductance, IR spectral data and UV-Visible. The results suggested that the
ligand HSBIBT bonded to the metal through N atom and square planner geometries were assigned
for the complexes.
Synthesis and Pharmacological Evaluation of Novel Heterocyclic CompoundIJSRD
2-[(4-bromo anilino)]-4-chloro-6-morpholino-1,3,5-triazine[2a] and 4-chloro-N-(4-fluorophenyl)-6-morpholino-1,3,5-triazin-2-amine [2b]were synthesized and studied for their biological activity. These compounds were prepared by the condensation of 4-bromoaniline and 4-fluoroaniline with 4-(4,6-dichloro-1,3,5-triazin-2-yl) morpholine [1] which is prepared by the reaction between 2,4,6-trichloro-1,3,5-triazine and morpholine. All the compounds were characterized by elemental analysis and spectral studies.
In this work a new prodrug polymer was
prepared with two attachment groups (amid-ester), using di
functional spacer such as ethanol amine, which could react with
polyacrylic acid producing amide group, with remain ethanol
terminal group which could react with captopril acyl chloride,
producing ester group with extended the arm substituted drug to
improve the hydrolysis and to prevent the steric effect of polymer
chains. Many advantages enhanced the prodrug of polymer. The
prepared polymers were characterized by FTIR, 1H –NMR
spectroscopies. Controlled drug release was studied in different
pH values at 37℃, using UV. Spectra with comparing with
calibration curve. The modification percentage test was studied,and swelling percentage was calculated and all physical properties were observed.
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...IOSRJAC
This research includes synthesis of new heterocyclic derivatives of quinazolinone and studying the possibility for their application as surfactants. The preparation process started by the reaction of pentadecanoyl chloride with anthranilic acid gave 2-pentadecyl-4H-benzo[3,1]oxazin-4-one [1] which was used as starting material to synthesis some heterocyclic compounds by a reaction with nitrogen nucleophiles. Compound [1] as starting material reacted by three ways. The first way react Compound [1] with semicarbazide, thiosemicarbazide and phenylsemicarbazide in pyridine as solvent to obtained [1-(4-oxo-2- pentadecylquinazolin-3(4H)-yl) urea [2], thiourea [3], phenylthiourea [4] respectively]. The second way include the reaction of Compound [1] with 99% hydrazine hydrate to produce 3-amino-2-pentadecylquinazolin- 4(3H)-one [5], then converted to amino derivatives [6-8] by the reaction of Compound [5] with different halogenated compounds such as (benzoyl chloride, acetyl chloride and chloro acetyl chloride ) in DMF and pyridine as catalyst. The third way include the reaction of compound [1] with different substituted amine and amide compounds (thiourea, hydroxylamine hydrochloride, glycine, ammonium acetate and phenyl hydrazine) respectively to obtain derivatives of quinazoline [9-14]. The produced compounds [2,4,5,7 and 12] react with propylene oxide in different moles (n=3, 5 and7) to yield novel groups of nonionic compounds having a function as surface active agents. The surface active properties like surface tension and interfacial tension, wetting time, cloud point, emulsion stability, foam height and CMC of these compounds were measured and showed a pronounced surface activity, good emulsifying properties and highly foaming in some of these compounds. Newly synthesized compounds were identified via spectral methods; their [FTIR and some of them by 1HNMR, 13C-NMR] and measurements of some of its physical properties.
Chapter 13 Determination of riociguat using ninhydrin as a chromogen 2019Ratnakaram Venkata Nadh
A simple method is described to determine the amount of riociguat in bulk and tablet formulation by visible spectrophotometry. Formation of a chromophore with max of 597 nm, due to the reaction between the aromatic amine groups present on riociguat and ninhydrin in citric acid medium forms the basis for the current method. Extension of conjugation due to attachment of two ninhydrin molecules to a riociguat molecule explains the noticed high intensity as well as max of the generated chromophore. Current ICH guidelines were followed to validate the method. The obtained regression equation (y = 0.0316x+0.001) has a good correlation coefficient (> 0.999) in the studied range of 5.0-30.0 μg mL-1. Due to lack of separation steps in the method, it is found to be rapid as well as simple. The recovery levels of riociguat were in the range of 99.87 – 100.06.
Novel coumarin isoxazoline derivatives: Synthesis and study of antibacterial ...Ratnakaram Venkata Nadh
A highly efficient and mild protocol for the syntheses of ethyl-3-
[7-benzyloxy-4-methyl-2-oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-
isoxazole carboxylates and ethyl-3-[7-benzyloxy-3-chloro-4-methyl-2-
oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-isoxazole carboxylates in
good yields via [3 þ 2] cycloaddition of in situ–generated nitrile
oxides from 7-benzyloxy-4-methyl-coumarin hydroxymoylchlorides
and 7-benzyloxy-3-chloro-4-methyl-coumarin hydroxymoylchlorides
respectively with ethyl-3-aryl prop-2-enoate has been developed.
The new compounds are screened for antibacterial activity.
Natural Anthraquinone Synthesis and DART-MS Analysis/DatabasingSteven Augustin
Poster Presentation at 2015 Great Lakes and Central Region Joint Meeting of the American Chemical Society. Eastern Michigan University Graduate Research, Dr. Ruth Ann Armitage and Dr. Timothy Friebe, graduate advisers.
Targeted Intermediates of Eudesmic Acid: Synthesis and X-ray Investigationsijtsrd
it was carried out synthesis of esters and their dinitro derivatives of 3,4,5-trimethoxybenzoic (eudesmic) acid. Esterification of eudesmic acid carried out n absolute methanol or ethanol and corresponding methyl and ethyl 3,4,5-trimethoxybenzoates (2, 3) have been synthesized in good yields. It was revealed that nitration of these esters gives only dinitro products. The structure of the synthesized compounds of the methyl and ethyl 2,6-dinitro-3,4,5-trimethoxybenzoates (4, 5) was determined by X-ray diffraction analysis (XRD). In the asymmetric part of the crystal structures of 4, 5 one and two molecules are observed, respectively. In crystalline structures a flat nitro groups and carboxylic groups do not participate in the conjugation with aromatic rings. In the crystal structure of 4, an intermolecular C8-H...O9 hydrogen bond is observed, these H bonds link the molecules along the [010] axis. In the crystal structure of 5, intermolecular C9B-H...O4A and C10B-H...O8A hydrogen bonds form chains along the [011] axis. The formed chains are cross linked by the intermolecular C9B-H...O5A hydrogen bonds. Olimova M.I. | Okmanov R. Ya. | Elmuradov B. Zh."Targeted Intermediates of Eudesmic Acid: Synthesis and X-ray Investigations" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-1 | Issue-6 , October 2017, URL: http://www.ijtsrd.com/papers/ijtsrd2417.pdf http://www.ijtsrd.com/chemistry/other/2417/targeted-intermediates-of-eudesmic-acid--synthesis-and-x-ray-investigations/olimova-mi
STUDIES ON TREATMENT OF PHARMACEUTICAL WASTE EFFLUENTS BY POLYMER MATERIALS M...EDITOR IJCRCPS
In the present study, sorption technique was used to achieve the optimum recovery of the pharmaceutical waste from effluents.
The modified urea formaldehyde resin was prepared and mixed with inorganic adsorbent at various proportions. The removal
capabilities of pharmaceutical waste by the prepared composite materials were investigated. Different factors affecting the uptake
such as contact time, pH value and aqueous volume to resin weight ratio have been investigated. The reaction mechanisms and
the optimum conditions for the treatment were deduced in the light of the obtained results.
Keywords: Sorption technique, Pharmaceutical waste, Different factors.
Determination of Riociguat by Oxidative Coupling Using Visible SpectrophotometryRatnakaram Venkata Nadh
A simple spectrophotometric method was developed to determine riociguat in bulk and tablet formulation. The present method lies on the oxidation of MBTH by Fe+3 ions in acidic medium to form active coupling species and followed by its coupling with riociguat to form the chromophore having lmax 660 nm. Validated the proposed method as per the existing guidelines of ICH. Good linearity (r~ 0.999) was observed for calibration curve in the studied concentration range (6.25 – 37.50 μg mL-1). Reproducibility, accuracy and precision of the method were confirmed from low values of % RSD.
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...IOSRJAC
There is a vast variety of naturally occurring glycosides which have marked pharmacological properties. These glycosides have widely diversed functional groups modifications which result in influencing pharmacological performance of corresponding glycosides. The 3,6-disubstituted-s-triazolo[3,4- b][1,3,4]thiadiazoles were glucosidated with 2,3,4,6tetra-o-acetyl α D glulopryanosyl bromide using simple methodologies. The compounds obtained in good yield in a 80-90 minutes.
Dynamic and Equilibrium Studies on the sorption of Basic dye (Basic Brown 4) ...madlovescience
Dynamic and Equilibrium Studies on the sorption of Basic dye (Basic Brown 4) onto Multi-walled Carbon Nanotubes Prepared from Renewable Carbon Precursors
Physical and Structural Characterization of Biofield Treated Imidazole Deriva...albertdivis
The Aim of present study was to evaluate the impact of biofield treatment on two imidazole derivatives (i.e., imidazole and 2-methylimidazole) by various analytical methods.
A STUDY TO EVALUATE THE IN VITRO ANTIMICROBIAL ACTIVITY AND ANTIANDROGENIC E...Dr. Pradeep mitharwal
The present paper deals with synthesis and characterization
of some new chromium (III) Schiff base complexes using microwave irradiation
technique as well as conventional heating. The S∩N donor benzothiazolines, 1-
(2-furanyl) ethanone benzothiazoline (Bzt1N
∩
SH), 1-(2-thienyl) ethanone
benzothiazoline (Bzt2N
∩
SH) and 1-(2-pyridyl) ethanone benzothiazoline
(Bzt3N
∩
SH) were prepared by the condensation of ortho-aminothiophenol with
respective ketones in ethanol.
Chapter 13 Determination of riociguat using ninhydrin as a chromogen 2019Ratnakaram Venkata Nadh
A simple method is described to determine the amount of riociguat in bulk and tablet formulation by visible spectrophotometry. Formation of a chromophore with max of 597 nm, due to the reaction between the aromatic amine groups present on riociguat and ninhydrin in citric acid medium forms the basis for the current method. Extension of conjugation due to attachment of two ninhydrin molecules to a riociguat molecule explains the noticed high intensity as well as max of the generated chromophore. Current ICH guidelines were followed to validate the method. The obtained regression equation (y = 0.0316x+0.001) has a good correlation coefficient (> 0.999) in the studied range of 5.0-30.0 μg mL-1. Due to lack of separation steps in the method, it is found to be rapid as well as simple. The recovery levels of riociguat were in the range of 99.87 – 100.06.
Novel coumarin isoxazoline derivatives: Synthesis and study of antibacterial ...Ratnakaram Venkata Nadh
A highly efficient and mild protocol for the syntheses of ethyl-3-
[7-benzyloxy-4-methyl-2-oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-
isoxazole carboxylates and ethyl-3-[7-benzyloxy-3-chloro-4-methyl-2-
oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-isoxazole carboxylates in
good yields via [3 þ 2] cycloaddition of in situ–generated nitrile
oxides from 7-benzyloxy-4-methyl-coumarin hydroxymoylchlorides
and 7-benzyloxy-3-chloro-4-methyl-coumarin hydroxymoylchlorides
respectively with ethyl-3-aryl prop-2-enoate has been developed.
The new compounds are screened for antibacterial activity.
Natural Anthraquinone Synthesis and DART-MS Analysis/DatabasingSteven Augustin
Poster Presentation at 2015 Great Lakes and Central Region Joint Meeting of the American Chemical Society. Eastern Michigan University Graduate Research, Dr. Ruth Ann Armitage and Dr. Timothy Friebe, graduate advisers.
Targeted Intermediates of Eudesmic Acid: Synthesis and X-ray Investigationsijtsrd
it was carried out synthesis of esters and their dinitro derivatives of 3,4,5-trimethoxybenzoic (eudesmic) acid. Esterification of eudesmic acid carried out n absolute methanol or ethanol and corresponding methyl and ethyl 3,4,5-trimethoxybenzoates (2, 3) have been synthesized in good yields. It was revealed that nitration of these esters gives only dinitro products. The structure of the synthesized compounds of the methyl and ethyl 2,6-dinitro-3,4,5-trimethoxybenzoates (4, 5) was determined by X-ray diffraction analysis (XRD). In the asymmetric part of the crystal structures of 4, 5 one and two molecules are observed, respectively. In crystalline structures a flat nitro groups and carboxylic groups do not participate in the conjugation with aromatic rings. In the crystal structure of 4, an intermolecular C8-H...O9 hydrogen bond is observed, these H bonds link the molecules along the [010] axis. In the crystal structure of 5, intermolecular C9B-H...O4A and C10B-H...O8A hydrogen bonds form chains along the [011] axis. The formed chains are cross linked by the intermolecular C9B-H...O5A hydrogen bonds. Olimova M.I. | Okmanov R. Ya. | Elmuradov B. Zh."Targeted Intermediates of Eudesmic Acid: Synthesis and X-ray Investigations" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-1 | Issue-6 , October 2017, URL: http://www.ijtsrd.com/papers/ijtsrd2417.pdf http://www.ijtsrd.com/chemistry/other/2417/targeted-intermediates-of-eudesmic-acid--synthesis-and-x-ray-investigations/olimova-mi
STUDIES ON TREATMENT OF PHARMACEUTICAL WASTE EFFLUENTS BY POLYMER MATERIALS M...EDITOR IJCRCPS
In the present study, sorption technique was used to achieve the optimum recovery of the pharmaceutical waste from effluents.
The modified urea formaldehyde resin was prepared and mixed with inorganic adsorbent at various proportions. The removal
capabilities of pharmaceutical waste by the prepared composite materials were investigated. Different factors affecting the uptake
such as contact time, pH value and aqueous volume to resin weight ratio have been investigated. The reaction mechanisms and
the optimum conditions for the treatment were deduced in the light of the obtained results.
Keywords: Sorption technique, Pharmaceutical waste, Different factors.
Determination of Riociguat by Oxidative Coupling Using Visible SpectrophotometryRatnakaram Venkata Nadh
A simple spectrophotometric method was developed to determine riociguat in bulk and tablet formulation. The present method lies on the oxidation of MBTH by Fe+3 ions in acidic medium to form active coupling species and followed by its coupling with riociguat to form the chromophore having lmax 660 nm. Validated the proposed method as per the existing guidelines of ICH. Good linearity (r~ 0.999) was observed for calibration curve in the studied concentration range (6.25 – 37.50 μg mL-1). Reproducibility, accuracy and precision of the method were confirmed from low values of % RSD.
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...IOSRJAC
There is a vast variety of naturally occurring glycosides which have marked pharmacological properties. These glycosides have widely diversed functional groups modifications which result in influencing pharmacological performance of corresponding glycosides. The 3,6-disubstituted-s-triazolo[3,4- b][1,3,4]thiadiazoles were glucosidated with 2,3,4,6tetra-o-acetyl α D glulopryanosyl bromide using simple methodologies. The compounds obtained in good yield in a 80-90 minutes.
Dynamic and Equilibrium Studies on the sorption of Basic dye (Basic Brown 4) ...madlovescience
Dynamic and Equilibrium Studies on the sorption of Basic dye (Basic Brown 4) onto Multi-walled Carbon Nanotubes Prepared from Renewable Carbon Precursors
Physical and Structural Characterization of Biofield Treated Imidazole Deriva...albertdivis
The Aim of present study was to evaluate the impact of biofield treatment on two imidazole derivatives (i.e., imidazole and 2-methylimidazole) by various analytical methods.
A STUDY TO EVALUATE THE IN VITRO ANTIMICROBIAL ACTIVITY AND ANTIANDROGENIC E...Dr. Pradeep mitharwal
The present paper deals with synthesis and characterization
of some new chromium (III) Schiff base complexes using microwave irradiation
technique as well as conventional heating. The S∩N donor benzothiazolines, 1-
(2-furanyl) ethanone benzothiazoline (Bzt1N
∩
SH), 1-(2-thienyl) ethanone
benzothiazoline (Bzt2N
∩
SH) and 1-(2-pyridyl) ethanone benzothiazoline
(Bzt3N
∩
SH) were prepared by the condensation of ortho-aminothiophenol with
respective ketones in ethanol.
New Schiff base ligand (E)-6-(2-(4-
(dimethylamino)benzylideneamino)-2-phenylacetamido)-3,3-
dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic
acid = (HL) Figure(1) was prepared via condensation of
Ampicillin and 4(dimethylamino)benzaldehyde in methanol
.Polydentate mixed ligand complexes were obtained from 1:1:2
molar ratio reactions with metal ions and HL, 2NA on reaction
with MCl2 .nH2O salt yields complexes corresponding to the
formulas [M(L)(NA)2Cl] ,where M =
Fe(II),Co(II),Ni(II),Cu(II),and Zn(II) and NA=nicotinamide.
The 1H-NMR, FT-IR, UV-Vis and elemental analysis
were used for the characterization of the ligand. The complexes
were structurally studied through AAS, FT-IR, UV-Vis,
chloride contents, conductance, and magnetic susceptibility
measurements. All complexes are non-electrolytes in DMSO
solution. Octahedral geometries have been suggested for each
of the complexes. The Schiff base ligands function as
tridentates and the deprotonated enolic form is preferred for
coordination. In order to evaluate the effect of the bactericidal
activity, these synthesized complexes, in comparison to the un
complexed Schiff base has been screened against bacterial
species, Staphy
Visible Spectrophotometric Determination of Gemigliptin Using Charge Transfer...Ratnakaram Venkata Nadh
A visible spectrophotometric method was developed and validated for the determination of gemigliptin present in bulk drug and tablet formulation. It involves an indirect method of charge transfer complex formation in presence of NBS, metol and suphanilic acid. Gemigliptin was subjected to oxidation with excess amount of oxidant (NBS) and the unconsumed NBS oxidizes metol to give p-N-methylbenzoquinone monoamine (PNMM) which in turn forms a charge transfer complex with sulphanilic acid. Then validated the above developed method as per the current ICH guidelines. An excellent correlation coefficient (> 0.999) was found for the obtained regression equation
(y = –0.0302x + 0.928) in the range of 2.0–30.0 μg mL-1. The method was found to be simple and rapid because it does not involve any solvent extraction. The recovery levels of the drug were in the range 99.92 – 100.08.
Visible Spectrophotometric Determination of Gemigliptin Using Charge Transfer...Ratnakaram Venkata Nadh
A visible spectrophotometric method was developed and validated for the determination of gemigliptin present in bulk drug and tablet formulation. It involves an indirect method of charge transfer complex formation in presence of NBS, metol and suphanilic acid. Gemigliptin was subjected to oxidation with excess amount of oxidant (NBS) and the unconsumed NBS oxidizes metol to give p-N-methylbenzoquinone monoamine (PNMM) which in turn forms a charge transfer complex with sulphanilic acid. Then validated the above developed method as per the current ICH guidelines. An excellent correlation coefficient (> 0.999) was found for the obtained regression equation
(y = –0.0302x + 0.928) in the range of 2.0–30.0 μg mL-1. The method was found to be simple and rapid because it does not involve any solvent extraction. The recovery levels of the drug were in the range 99.92 – 100.08.
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.
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, Characterization, and Antibacterial Activity of Some Novel 5-Chlor...IJERA Editor
The development of potential antibacterial requires the synthesis of a new series of 5- Chloroisatin derivatives incorporating various aromatic aldehydes in the case 1,3-Dipolar Cycloaddition including Nitrile oxide, as well as the cycloaddition Alcyne-Azide Catalytic with Copper. The charcterization of the structure of the synthesized compounds was confirmed by means of their IR, 1H-NMR and 13C-NMR spectral data. In addition, the antibacterial properties in vitro were tested against certain microorganisms using the disk diffusion technique. A majority of compounds show better activity against several of the microorganisms.
The Eco-friendly Marine Gastropod Turbo brunneus (L. 1758) and its Vital role...rahulmonikasharma
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
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• Remote control system for accessing CCR and allied system over serial or TCP.
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Technical Specifications
Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
Key Features
Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
• Remote control: Parallel or serial interface
• Compatible with MAFI CCR system
• Copatiable with IDM8000 CCR
• Compatible with Backplane mount serial communication.
• Compatible with commercial and Defence aviation CCR system.
• Remote control system for accessing CCR and allied system over serial or TCP.
• Indigenized local Support/presence in India.
Application
• Remote control: Parallel or serial interface.
• Compatible with MAFI CCR system.
• Compatible with IDM8000 CCR.
• Compatible with Backplane mount serial communication.
• Compatible with commercial and Defence aviation CCR system.
• Remote control system for accessing CCR and allied system over serial or TCP.
• Indigenized local Support/presence in India.
• Easy in configuration using DIP switches.
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Synthesis and Characterization of a New Cationic Surfactant Derived from 5-Chloro-1H-indole-2,3-dione In Aqueous Systems
1. Z. Tribak. et al. Int. Journal of Engineering Research and Application www.ijera.com
ISSN : 2248-9622, Vol. 7, Issue 4, ( Part -1) April 2017, pp.04-08
www.ijera.com DOI: 10.9790/9622-0704010408 4 | P a g e
Synthesis and Characterization of a New Cationic Surfactant
Derived from 5-Chloro-1H-indole-2,3-dione In Aqueous Systems
Z. Tribak1
, R. Ghibate5
, M.K. Skalli1
, Y. Kandri Rodi2
, D. Mrani3
, A. Aouniti4
,
B. Hammouti4
, O. Senhaji5*
1
Laboratory of Applied Chemistry, Sidi Mohamed Ben Abdellah University, Faculty of Science and Technology
of Fez, Morocco.
2
Laboratory of Applied Organic Chemistry, Sidi Mohamed Ben Abdellah University, Faculty of Science and
Technology of Fez, Morocco.
3
Laboratory of Analytical Chemistry, Environment and Materials(ACEM),Moulay Ismail University, Faculty of
Science and Technology of Erracchidia, Morocco.
4
LCAE-URAC18, Faculty of Science, Mohammed first University, Po Box 717, 60000 Oujda, Morocco.
5
Laboratory of Applied Physical Chemistry (ECPA), MoulayIsmaïl University, Faculty of Sciences and
Technology of Erracchidia, Morocco.
ABSTRACT:In this paper, anovel cationic surfactant is synthesized by the alkylation reaction of 5-Chloro-
1H-indole-2,3-dioneunder the conditions of phase transfer catalysis and quaternizationby trimethylamine in
acetone solution.Chemical structures of synthesized compounds were confirmed by 1
HNMR and 13
C NMR. The
micellization of cationic surfactant in aqueous solution at room temperature has been reported using the
conductivity of the measurements
Keywords:5-Chloro-1H-indole-2,3-dione, alkylation, quaternization, monomer, surfactants
I. INTRODUCTION
The particular structure of the surfactants
allows them to be classified among the molecules
most present in the cosmetics, pharmaceutical or
agroalimentary industries [1]. The high production
volumes of these industries have highlighted the
need to use non-polluting surfactants, which can be
synthetic or natural. This current problem has
resulted in the use of agro-resources such as
carbohydrates, phosphonates [2] and 5-Chloroisatin
derivatives as a starting material for the synthesis of
compounds with high added value.In the literature,
5-chloro-1H-indole-2,3-dione is a polyvalent
chemical building block capable of forming a large
number of heterocyclic molecules [3]. The
compound has an indole ring structure common to
many pharmaceutical products. Its derivatives have
exhibited activities such as antibacterial [4], anti-
inflammatory [5], analgesic [6], anti-viral [7],
antifungal [8], anti-tubercular [9], anti-depressant
[10] and anticorrosive [11]. The presence of several
reaction centers in isatin and its derivatives makes
them capable of participating in a large number of
reactions [12].The keto group at position 2 and in
particular at position 3 can be added to the C-O bond
and condensation reactions [13].Through the
primary amine group, compounds of the 5-
Chloroisatin series are able to penetrate N-alkylation
and thereafterquaternization by trimethylamine as an
example in the case of the synthesis of the novel
surfactants ofindole [14].Generally, the structure of a
surfactant is said to be amphiphilic, it is defined by
the joint presence of a hydrophilic part and a
hydrophobic part, depending on the nature of the
hydrophilic part, cationic, anionic or zwitterionic
surfactants may be found or nonionic surfactants
[15-18]. The hydrophobic part, for its part, is most
often in the form of a carbon chain of variable
length, whether branched or not. It is well known
that surfactant molecules are associated with
micelles which begin to form above the critical
micellar concentration (CMC) [19-22]. Numerous
factors such as the addition of electrolytes [23-25],
the pH of the buffer [26], the temperature [27,28],
the addition of organic modifiers [29, 30] Ionic
strength of the aqueous solution [31, 32], the
presence of additives etc., make this value different
from that determined in pure water.The
determination of the CMC takes place in several
ways such as the tensiometry which records the
decrease in the surface tension as a function of the
surfactant concentrations up to a limit beyond which
the surface tension no longer decreases, and other
methods used as conductivity [33-34] for charged
surfactants, spectrofluorometry, nuclear magnetic
resonance and UV-visible absorption spectroscopy
[35-37].In the present work, we describe the
synthesis of a new surfactant monomer derived from
5-Chloroisatin via the N-alkylation method under the
conditions of phase transfer catalysis followed by
the quaternizationof 1- (6-bromohexyl) 5-
chloroindoline-2,3-dione, with trimethylamine. The
RESEARCH ARTICLE OPEN ACCESS
2. Z. Tribak. et al. Int. Journal of Engineering Research and Application www.ijera.com
ISSN : 2248-9622, Vol. 7, Issue 4, ( Part -1) April 2017, pp.04-08
www.ijera.com DOI: 10.9790/9622-0704010408 5 | P a g e
structures of the compounds are perfectly packaged
by 1
H NMR, 13
C NMR. The critical micelle
concentration of our surfactant was determined in
pure water at 25 °C by a conductimeter.
II. RESULTS AND DISCUSSION
Preparation of 1- (6-bromohexyl) -5-
chloroindoline-2,3-dione:
In order to obtain novel heterocyclic
compounds having the 5-chloro-1H-indole-2,3-dione
nucleus [38], we were interested in the condensation
of 5-Chloroisatin (1)with the 1,6-dibromohexane,
under the conditions of phase transfer catalysis
(CTP)[39], solubilizing in N, N-dimethylformamide
(DMF) in the presence of a weak base and a catalyst
to promote the reaction. After purification by
chromatography on a silica column with a mixture of
ethyl acetate/hexane [40], the 1- (6-bromohexyl) -5-
chloroindoline-2,3-dione (2) compound is obtained
in good yield.
Figure 1: Synthesis of novel derivatives of 5-Chloro-1H-indole-2,3-dione
Quaternization of 1- (6-bromohexyl) -5-
chloroindoline-2,3-dione(3):
Quaternization of 1- (6-bromohexyl) -5-
chloroindoline-2,3-dione, is obtained by
trimethylamine [41] solubilized in acetone at room
temperature, according to the following reaction:
Figure2: Synthesis of novel cationic surfactant.
The product obtained is purified by precipitation in
diethyl ether with a yield of 95% and it’s soluble in
methanol and water.
CMC determination:
With the intention of estimating the CMC of
our cationic surfactant, the conductivity plots were
carried out as a function of the concentration of 5-
chloro-1-(6-(trimethyl-𝜆4
-azanyl)hexyl)indoline-2,3-
dione in an aqueous solution at room temperature[42].
Measurements for selected surfactants were carried
out in pure water and at different concentrations of 5-
chloro-1-(6-(trimethyl-𝜆4
-azanyl)hexyl)indoline-2,3-
dione at pH 7.0 and are shown in Table 1.The first
corresponds to the concentration range below the
CMC, when only the surfactant monomers exist in
solution [43].
At higher concentrations of surfactant, the
micelles begin to form and a change in slope occurs
because the conductivity increases in a different
way.The intersection of these two lines is taken as the
CMC value of the surfactant. Indeed, at this CMC
concentration, many important properties of surfactant
usually change strongly in the solution [44-47]. The
critical micelle concentration was determined in pure
water at 25°C by means of conductometer and found
to be 5.10-3
M. The results are shown in Figure 3.
Table1: Variation of the specific conductivity relative to the surfactant concentration for the conductivity
determination of the CMC at T = 25°C. (pH 7.0).
C
(M) 1.25 10-3
2.5 10-3
5 10-3
10 10-3
13.3 10-3
20 10-3
𝛘
(mS) 91.2 175.2 350 652 875 1232
3. Z. Tribak. et al. Int. Journal of Engineering Research and Application www.ijera.com
ISSN : 2248-9622, Vol. 7, Issue 4, ( Part -1) April 2017, pp.04-08
www.ijera.com DOI: 10.9790/9622-0704010408 6 | P a g e
Figure 3: Variation of the conductivity of the surfactant with its concentration atambient temperature.
Experimental Part:
Melting points were determined by the
Kofler bench. NMR spectra were recorded on Bruker
300 NMR spectrometer advancement in CDCl3 using
tetramethylsilane (TMS) as reference, chemical shifts
are reported in parts per million of the inductive field.
The coupling constants (J) are in hertz. The following
abbreviations are used to describe peak models: s,
singlet; d, doublet; dd, double doublet; t, triplet; q,
quartet; m, multiplet. The conductivity has been
measured at 25 °C with a conductometer.
Synthesis of compound 2:
In a 100 ml two-necked flask, to a solution of
5-Chloro-1H-indole-2,3-dione (0.4 g, 2.20 mmol) in
DMF (15 ml), Potassium carbonate (0.5 g, 3.3 mmol),
a catalytic amount of tetra-n-butylammonium bromide
(0.1 g, 0.3 mmol) and the brominated reagent were
added. The mixture is activated by stirring for 48
hours at 25°C. After evaporation of the solvent and
treatment of the reaction, the crude reaction product is
purified by column chromatography. The new product
is isolated as a powder with good yield.
1- (6-bromohexyl) -5-chloroindoline-2,3-dione(2):
Yield: 74%;mp: 66-70°C; Rf = 0.8; RMN1
H (CDCl3;
300MHz): δ (ppm) 7.68 (dd, H, CHAr,J4
H-H = 1.5 Hz,
J3
H-H = 4.5 Hz) ; 7.60 (d, H, CHAr ,J4
H-H = 1.5 Hz);
7.24 (d, H, CHAr,J3
H-H = 6 Hz); 3.65 (t, 2H, CH2, J4
H-H
= 3Hz); 3.51 (t, 2H, CH2, J3
H-H= 6Hz); 1.73-1.82 (m,
2H, CH2), 1.54-1.63 (m, 2H, CH2) , 1.38-1.46(m, 4H,
CH2). RMN13
C (CDCl3; 75MHz): δ (ppm): 182.89
(C=O); 158.35 (N-C=O); 149.72, 127.72, 119.40(Cq);
137.39, 124.39, 112.88 (CHAr); 35.56, 32.58, 27.67,
27.00, 25.72(CH2).
Synthesis of compound (3):
In a 100 ml single-necked flask equipped
with a magnetic bar, 1 equivalent of 5-Chloroisatin
derivative in 15 ml of acetone is introduced and then 5
equivalents of trimethylamine (45% w/w) are added.
The mixture is stirred at room temperature; the
reaction is followed by thin layer chromatography
(TLC) every hour for about 24h. After a certain time,
the total disappearance of the starting bromide is seen.
At the end of the handling, the solvent is evaporated
under vacuum and the mixture treated. The precipitate
obtained is a slightly violet solid which is soluble in
the minimum of methanol and then purified by
precipitation in diethyl ether. The product is then
characterized by proton NMR, and carbon NMR.
5-chloro-1-(6-(trimethyl- 𝜆4
-azanyl)hexyl)indoline-
2,3-dione (3):
Yield: 88%;mp: 100-120°C; Rf= 0.6 ; RMN 1
H
(CDCl3; 300MHz) : δ (ppm) 7.35( d, H, HAr,4
JH-H =1.8
Hz); 7.17-7.2(dd H, HAr, 4
JH-H =3 Hz, 3
JH-H =9 Hz);
6.96(d, H, HAr,3
JH-H =9Hz); 3.52-3.71(m, 4H, CH2);
3.31(t, 2H, CH2, 3
JH-H=9Hz,4
JH-H =3Hz); 3.15-3.25(m,
2H, CH2); 1.57-1.64(m, 4H, CH2); 2.97(s, 9H,
CH3).RMN13
C (CDCl3; 75MHz): δ(ppm)
209.77(C=O); 177.99(N-C=O); 141.54, 131.28,
128.36(Cq); 130.03, 123.79, 111.10(CHAr); 26.06,
25.45, 25.05, 22.09(CH2), 29.83(CH3).
III. CONCLUSION
Our work was oriented on the synthesis study
and the characterization of a new cationic surfactant
derived from 5-Chloro-1H-indole-2,3-dione. The
production of this monomer takes place in two stages,
firstly the alkylation of 5-Chloroisatin with the
brominated reagent under the conditions of catalysis
by phase transfer and then the quaternization of 1- (6-
bromohexyl) -5-chloroindoline -2,3-dione, the
synthesized structures were identified on the basis of
the NMR spectral data. Tests of the conductimetric
method in water at ambient temperature made it
possible to study the behaviour of the micellization of
our cationic surfactant. Conductivity is a useful
technique for determining the thermodynamic
parameters of the surfactant micellization.
4. Z. Tribak. et al. Int. Journal of Engineering Research and Application www.ijera.com
ISSN : 2248-9622, Vol. 7, Issue 4, ( Part -1) April 2017, pp.04-08
www.ijera.com DOI: 10.9790/9622-0704010408 7 | P a g e
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