The document provides procedures for microscale synthesis of several organic compounds including aspirin, E-benzal, and azodyes. Microscale chemistry uses small quantities of chemicals to reduce waste and improve safety. It describes basic microscale equipment like conical vials, air condensers, Craig tubes for recrystallization, and pipettes. The aspirin synthesis involves reacting salicylic acid with acetyl chloride to form aspirin, which is then recrystallized. The E-benzal synthesis reacts benzaldehyde with hydroxylamine hydrochloride in the presence of sodium hydroxide.
Quinoxaline as a potent heterocyclic moietyiosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
1. The experiment aims to perform the assay of Ibuprofen as per Indian Pharmacopoeia.
2. Ibuprofen is titrated with 0.1M sodium hydroxide solution using phenolphthalein as indicator.
3. The percentage purity of Ibuprofen is calculated based on the titration results.
Practical Experiment 8: To synthesize and characterized barbaturic acid SONALI PAWAR
The document describes an experiment to prepare barbituric acid from urea and diethyl malonate. Sodium metal is reacted with ethanol to form sodium ethoxide, which promotes a condensation reaction between diethyl malonate and urea. This results in the cyclization and formation of barbituric acid. The theoretical yield is calculated to be 64g based on the reactants used. The actual yield obtained is 61g, giving a percentage yield of 95.3%.
Synthesis of at least two important members of the following groups of drugs: sulphonamides, antimalarials, antibiotics, barbiturates. adrenergic agents, antihistamines and antineoplastic agents.
This document summarizes the laboratory synthesis of triphenyl imidazole. It begins by stating the aim of synthesizing 2,4,5 triphenyl imidazole using benzil, ammonium acetate, benzaldehyde, and glacial acetic acid via the Debus-Radziszewski reaction. It then provides details on the synthesis of benzil as a starting material and the reaction mechanism. The procedure describes heating the reactants at 100°C for 3-4 hours to form an orange solution, cooling, neutralizing with ammonium hydroxide, and filtering and drying the precipitated triphenyl imidazole product.
Synthesis of drug & drug intermediates: Paracetamol b) Benzocaine c) Aspirin d) Phenacetin e) PABA (Para amino-benzoic acid f) Meta Nitro-benzaldehyde g) Ethyl para hydroxy-benzoate h) Para Amino phenol i) Methyl salicylate.
The document describes the synthesis of barbituric acid from diethyl malonate. It involves a Knoevenagel condensation reaction between sodium, ethyl malonate, and urea in absolute alcohol. The product, barbituric acid, is collected by filtration and crystallization. Barbituric acid is used as a sedative and hypnotic with potential overdose risks.
This document describes the synthesis of benzocaine from p-aminobenzoic acid. P-aminobenzoic acid is reacted with ethanol in the presence of hydrochloric acid via an esterification reaction to form ethyl p-aminobenzoate (benzocaine). The percentage yield of benzocaine obtained was 93.3%, close to the theoretical yield, and it has a melting point of 91°C. Benzocaine is used as a local anesthetic to relieve minor mouth pain.
Quinoxaline as a potent heterocyclic moietyiosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
1. The experiment aims to perform the assay of Ibuprofen as per Indian Pharmacopoeia.
2. Ibuprofen is titrated with 0.1M sodium hydroxide solution using phenolphthalein as indicator.
3. The percentage purity of Ibuprofen is calculated based on the titration results.
Practical Experiment 8: To synthesize and characterized barbaturic acid SONALI PAWAR
The document describes an experiment to prepare barbituric acid from urea and diethyl malonate. Sodium metal is reacted with ethanol to form sodium ethoxide, which promotes a condensation reaction between diethyl malonate and urea. This results in the cyclization and formation of barbituric acid. The theoretical yield is calculated to be 64g based on the reactants used. The actual yield obtained is 61g, giving a percentage yield of 95.3%.
Synthesis of at least two important members of the following groups of drugs: sulphonamides, antimalarials, antibiotics, barbiturates. adrenergic agents, antihistamines and antineoplastic agents.
This document summarizes the laboratory synthesis of triphenyl imidazole. It begins by stating the aim of synthesizing 2,4,5 triphenyl imidazole using benzil, ammonium acetate, benzaldehyde, and glacial acetic acid via the Debus-Radziszewski reaction. It then provides details on the synthesis of benzil as a starting material and the reaction mechanism. The procedure describes heating the reactants at 100°C for 3-4 hours to form an orange solution, cooling, neutralizing with ammonium hydroxide, and filtering and drying the precipitated triphenyl imidazole product.
Synthesis of drug & drug intermediates: Paracetamol b) Benzocaine c) Aspirin d) Phenacetin e) PABA (Para amino-benzoic acid f) Meta Nitro-benzaldehyde g) Ethyl para hydroxy-benzoate h) Para Amino phenol i) Methyl salicylate.
The document describes the synthesis of barbituric acid from diethyl malonate. It involves a Knoevenagel condensation reaction between sodium, ethyl malonate, and urea in absolute alcohol. The product, barbituric acid, is collected by filtration and crystallization. Barbituric acid is used as a sedative and hypnotic with potential overdose risks.
This document describes the synthesis of benzocaine from p-aminobenzoic acid. P-aminobenzoic acid is reacted with ethanol in the presence of hydrochloric acid via an esterification reaction to form ethyl p-aminobenzoate (benzocaine). The percentage yield of benzocaine obtained was 93.3%, close to the theoretical yield, and it has a melting point of 91°C. Benzocaine is used as a local anesthetic to relieve minor mouth pain.
B. Pharm. (Honours) Part-IV Practical, Medicinal Chemistry-II, MANIKImran Nur Manik
2. Medicinal Chemistry-II: (Marks-30)
Synthesis of at least two important members of the following groups of drugs: sulphonamides, antimalarials, antibiotics, barbiturates. adrenergic agents, antihistamines and antineoplastic agents.
Synthesis of 7 hydroxy-4-methyl coumarinkiran2mane
This document describes the synthesis of 7-hydroxy-4-methyl coumarin via the Pechmann reaction. The Pechmann reaction involves the condensation of resorcinol with ethyl acetoacetate in concentrated sulfuric acid. The reaction mechanism proceeds through the initial formation of a β-hydroxy ester intermediate, which then cyclizes and dehydrates to form the coumarin product. Following the described procedure yields 4.3g of a pale yellow solid product, which is 49% of the theoretical yield. Characterization by TLC shows the product has a different Rf value than the starting materials, indicating formation of 7-hydroxy-4-methyl coumarin.
Practical Experiment 1: Benzimidazole from orthophenylene diamine SONALI PAWAR
The document describes the synthesis of benzimidazole from orthophenylene diamine (OPD). Orthophenylene diamine and formic acid are heated together in a condensation reaction to form benzimidazole. The theoretical yield of benzimidazole is calculated and the practical yield is measured to be 98.64% with a melting point of 170-175°C. Benzimidazole is then characterized.
Analysis of analgesics and antipyretics.induhdghcfgfgftf
The document summarizes analytical methods for several analgesics and antipyretics. It discusses classification of analgesics and antipyretics and their mechanisms of action. Specific analytical methods covered include titrimetric, spectrophotometric, chromatographic and colorimetric assays for drugs like aspirin, diclofenac sodium, aceclofenac, ibuprofen, paracetamol, analgin and antipyrine. Gravimetric, colorimetric and polarographic methods are described for the analysis of antipyrine.
The document describes a two-step process to prepare benzocaine from p-nitrobenzoic acid. The first step involves reducing p-nitrobenzoic acid to p-aminobenzoic acid using tin and hydrochloric acid. The second step is a Fischer esterification of p-aminobenzoic acid with ethanol in the presence of sulfuric acid to form benzocaine. The procedure provides details of the reaction conditions and calculations to determine the theoretical and percent yield of benzocaine produced.
The document describes a two-step process to prepare 2-phenylindole from phenylhydrazine and acetophenone. The first step involves a condensation reaction of acetophenone and phenylhydrazine in ethanol and acetic acid to form acetophenone phenylhydrazone. The second step performs a Fischer indole cyclization of acetophenone phenylhydrazone in phosphoric acid and sulfuric acid to yield the final product 2-phenylindole. The product is then purified through recrystallization and its melting point is obtained.
1) The document describes an experiment to synthesize benzocaine from p-amino benzoic acid through an esterification reaction.
2) P-amino benzoic acid, ethanol, sulfuric acid, and sodium carbonate are reacted through refluxing.
3) Thin layer chromatography is used to analyze the reaction product and confirms benzocaine formation by its different Rf value from the starting material p-amino benzoic acid.
Phenytoin is synthesized from benzil in a multi-step reaction involving a pinacol rearrangement. Benzil and urea are condensed in the presence of base to form an intermediate 1,2-diol, which is then protonated to form an oxonium ion. Dehydration leads to a carbonium ion that undergoes a 1,2 shift of the phenyl ring to form a phenonium ion. Rearrangement of this ion generates the final product, phenytoin, which is isolated by acidification and recrystallization with a 91.4% yield.
Here, you find out the
Requirements for preparation of benzimidazole
Synthetic reaction of benzimidazole
Theory regarding benzimidazole
Procedure for preparation of benzimidazole
Observation and calculations
Result or report
This document describes the preparation of p-bromoaniline from acetanilide. It involves a two step process:
1. Bromination of acetanilide using potassium bromate and potassium bromide in the presence of tartaric acid yields p-bromoacetanilide as the major product.
2. Hydrolysis of p-bromoacetanilide using hydrochloric acid and heat produces p-bromoaniline. The product is isolated by adjusting the pH to basic and cooling.
Yields, melting points and reactions are calculated and mechanisms are provided for both steps. Chemical tests to identify the products are also outlined.
The document summarizes an organic chemistry experiment involving a multi-step synthesis of benzilic acid from benzaldehyde. The synthesis proceeded in three steps: (1) benzaldehyde was condensed to form benzoin, (2) benzoin was oxidized to form benzil, and (3) benzil underwent rearrangement and acidification to form benzilic acid. While product yields were high between 98-86%, melting points were lower than expected, possibly due to experimental errors. NMR spectroscopy confirmed the structure of the final product, benzilic acid.
The document summarizes the multistep synthesis of 2,6-bis(benzylidene)cyclohexanone. The first steps involve synthesizing the starting materials - cyclohexanone from cyclohexene and benzaldehyde from benzene. Cyclohexanone is made through oxidation of cyclohexanol, which is obtained by acid-catalyzed hydration of cyclohexene. Benzaldehyde is prepared by bromination of benzene to form bromobenzene, followed by preparation of phenylmagnesium bromide and carbonation to yield benzaldehyde. Finally, an Aldol condensation of cyclohexanone and benzaldehyde under basic conditions produces the target compound 2,
This document summarizes the synthesis of 7-Hydroxy-4-Methyl Coumarin via the Pechmann condensation reaction of resorcinol and ethyl acetoacetate in the presence of concentrated sulfuric acid. Coumarins are an important class of compounds that are found in plants and have various medical applications such as antimicrobial and antitumor properties. The procedure involves cooling concentrated sulfuric acid to below 5°C and adding a solution of resorcinol and ethyl acetoacetate dropwise, followed by workup to obtain an impure product that is recrystallized from ethanol.
The document describes the synthesis of hexaammine cobalt(III) chloride from cobalt(II) chloride hexahydrate. Cobalt(II) is oxidized to cobalt(III) using air and activated carbon as a catalyst. The product is purified by recrystallization and characterized using IR spectroscopy. A 79.1% yield of the orange product was obtained, which matches literature values. The experiment provides students hands-on experience in synthesizing and characterizing a coordination compound.
B. Pharm. (Honours) Part-III Practical, Medicinal Chemistry,ManikImran Nur Manik
Synthesis of drug & drug intermediates: Paracetamol b) Benzocaine c) Aspirin d) Phenacetin e) PABA (Para amino-benzoic acid f) Meta Nitro-benzaldehyde g) Ethyl para hydroxy-benzoate h) Para Amino phenol i) Methyl salicylate.
1) The document describes the procedure for synthesizing benzimidazole from o-phenylenediamine and formic acid.
2) Key steps include heating a mixture of o-phenylenediamine and excess formic acid at 100°C for 2 hours, then making the reaction mixture alkaline with sodium hydroxide to precipitate crude benzimidazole.
3) Benzimidazole has biological applications as an active component in anthelmintic and antiulcer drugs, and its derivatives also show antimicrobial and anticancer properties.
This document describes the procedure for preparing adipic acid from cyclohexanol via oxidation. Cyclohexanol is oxidized using nitric acid and ammonium metavanadate catalyst at 65-70°C to yield adipic acid crystals. The theoretical and experimental yields and melting point of adipic acid are calculated and measured. Adipic acid is an important industrial dicarboxylic acid used to produce nylon polymers.
This document describes the preparation of p-nitro acetanilide from acetanilide. Acetanilide is nitrated using nitric and sulfuric acid. This produces p-nitro acetanilide as the major product along with a minor amount of o-nitro acetanilide. The p-nitro acetanilide product is purified by recrystallization from ethanol, yielding colorless crystals. Percent yield of the product is calculated and the melting point is obtained and compared to literature values.
This document describes the synthesis of benzanilide from aniline via a Schotten-Baumann reaction. Aniline reacts with benzoyl chloride in the presence of sodium hydroxide to form benzanilide and hydrochloric acid. The reaction involves benzoylation, where the benzoyl group is inserted in place of the active hydrogen on the amine group of aniline. Details of the reaction mechanism, chemicals used, equipment needed and procedure for synthesizing benzanilide are provided. The theoretical and percent yields are also calculated.
Wear gloves and safety goggles. Work in the fume hood.
Procedure:
1. Dissolve benzaldehyde (208 mg, 2 mmol) in ethanol (2 mL) in a test tube.
2. In a separate test tube, dissolve hydroxylamine hydrochloride (189 mg, 2.4 mmol) in ethanol (2 mL).
3. Slowly add the hydroxylamine hydrochloride solution to the benzaldehyde solution with stirring.
4. Add sodium hydroxide pellets (140 mg, 3.5 mmol) and stir until reaction is complete.
5. Extract the product by adding diethyl ether (2 mL) and collecting the ether layer.
This document describes an experiment to synthesize aspirin. Students will learn the process of preparing aspirin through acetylation of salicylic acid with acetic anhydride. They will purify the product and test for the absence of salicylic acid using ferric chloride to form complexes. The history of aspirin's development is outlined from its identification in willow bark to its commercial production. Aspirin's structure and the two-step industrial synthesis from phenol and carbon dioxide is also summarized.
B. Pharm. (Honours) Part-IV Practical, Medicinal Chemistry-II, MANIKImran Nur Manik
2. Medicinal Chemistry-II: (Marks-30)
Synthesis of at least two important members of the following groups of drugs: sulphonamides, antimalarials, antibiotics, barbiturates. adrenergic agents, antihistamines and antineoplastic agents.
Synthesis of 7 hydroxy-4-methyl coumarinkiran2mane
This document describes the synthesis of 7-hydroxy-4-methyl coumarin via the Pechmann reaction. The Pechmann reaction involves the condensation of resorcinol with ethyl acetoacetate in concentrated sulfuric acid. The reaction mechanism proceeds through the initial formation of a β-hydroxy ester intermediate, which then cyclizes and dehydrates to form the coumarin product. Following the described procedure yields 4.3g of a pale yellow solid product, which is 49% of the theoretical yield. Characterization by TLC shows the product has a different Rf value than the starting materials, indicating formation of 7-hydroxy-4-methyl coumarin.
Practical Experiment 1: Benzimidazole from orthophenylene diamine SONALI PAWAR
The document describes the synthesis of benzimidazole from orthophenylene diamine (OPD). Orthophenylene diamine and formic acid are heated together in a condensation reaction to form benzimidazole. The theoretical yield of benzimidazole is calculated and the practical yield is measured to be 98.64% with a melting point of 170-175°C. Benzimidazole is then characterized.
Analysis of analgesics and antipyretics.induhdghcfgfgftf
The document summarizes analytical methods for several analgesics and antipyretics. It discusses classification of analgesics and antipyretics and their mechanisms of action. Specific analytical methods covered include titrimetric, spectrophotometric, chromatographic and colorimetric assays for drugs like aspirin, diclofenac sodium, aceclofenac, ibuprofen, paracetamol, analgin and antipyrine. Gravimetric, colorimetric and polarographic methods are described for the analysis of antipyrine.
The document describes a two-step process to prepare benzocaine from p-nitrobenzoic acid. The first step involves reducing p-nitrobenzoic acid to p-aminobenzoic acid using tin and hydrochloric acid. The second step is a Fischer esterification of p-aminobenzoic acid with ethanol in the presence of sulfuric acid to form benzocaine. The procedure provides details of the reaction conditions and calculations to determine the theoretical and percent yield of benzocaine produced.
The document describes a two-step process to prepare 2-phenylindole from phenylhydrazine and acetophenone. The first step involves a condensation reaction of acetophenone and phenylhydrazine in ethanol and acetic acid to form acetophenone phenylhydrazone. The second step performs a Fischer indole cyclization of acetophenone phenylhydrazone in phosphoric acid and sulfuric acid to yield the final product 2-phenylindole. The product is then purified through recrystallization and its melting point is obtained.
1) The document describes an experiment to synthesize benzocaine from p-amino benzoic acid through an esterification reaction.
2) P-amino benzoic acid, ethanol, sulfuric acid, and sodium carbonate are reacted through refluxing.
3) Thin layer chromatography is used to analyze the reaction product and confirms benzocaine formation by its different Rf value from the starting material p-amino benzoic acid.
Phenytoin is synthesized from benzil in a multi-step reaction involving a pinacol rearrangement. Benzil and urea are condensed in the presence of base to form an intermediate 1,2-diol, which is then protonated to form an oxonium ion. Dehydration leads to a carbonium ion that undergoes a 1,2 shift of the phenyl ring to form a phenonium ion. Rearrangement of this ion generates the final product, phenytoin, which is isolated by acidification and recrystallization with a 91.4% yield.
Here, you find out the
Requirements for preparation of benzimidazole
Synthetic reaction of benzimidazole
Theory regarding benzimidazole
Procedure for preparation of benzimidazole
Observation and calculations
Result or report
This document describes the preparation of p-bromoaniline from acetanilide. It involves a two step process:
1. Bromination of acetanilide using potassium bromate and potassium bromide in the presence of tartaric acid yields p-bromoacetanilide as the major product.
2. Hydrolysis of p-bromoacetanilide using hydrochloric acid and heat produces p-bromoaniline. The product is isolated by adjusting the pH to basic and cooling.
Yields, melting points and reactions are calculated and mechanisms are provided for both steps. Chemical tests to identify the products are also outlined.
The document summarizes an organic chemistry experiment involving a multi-step synthesis of benzilic acid from benzaldehyde. The synthesis proceeded in three steps: (1) benzaldehyde was condensed to form benzoin, (2) benzoin was oxidized to form benzil, and (3) benzil underwent rearrangement and acidification to form benzilic acid. While product yields were high between 98-86%, melting points were lower than expected, possibly due to experimental errors. NMR spectroscopy confirmed the structure of the final product, benzilic acid.
The document summarizes the multistep synthesis of 2,6-bis(benzylidene)cyclohexanone. The first steps involve synthesizing the starting materials - cyclohexanone from cyclohexene and benzaldehyde from benzene. Cyclohexanone is made through oxidation of cyclohexanol, which is obtained by acid-catalyzed hydration of cyclohexene. Benzaldehyde is prepared by bromination of benzene to form bromobenzene, followed by preparation of phenylmagnesium bromide and carbonation to yield benzaldehyde. Finally, an Aldol condensation of cyclohexanone and benzaldehyde under basic conditions produces the target compound 2,
This document summarizes the synthesis of 7-Hydroxy-4-Methyl Coumarin via the Pechmann condensation reaction of resorcinol and ethyl acetoacetate in the presence of concentrated sulfuric acid. Coumarins are an important class of compounds that are found in plants and have various medical applications such as antimicrobial and antitumor properties. The procedure involves cooling concentrated sulfuric acid to below 5°C and adding a solution of resorcinol and ethyl acetoacetate dropwise, followed by workup to obtain an impure product that is recrystallized from ethanol.
The document describes the synthesis of hexaammine cobalt(III) chloride from cobalt(II) chloride hexahydrate. Cobalt(II) is oxidized to cobalt(III) using air and activated carbon as a catalyst. The product is purified by recrystallization and characterized using IR spectroscopy. A 79.1% yield of the orange product was obtained, which matches literature values. The experiment provides students hands-on experience in synthesizing and characterizing a coordination compound.
B. Pharm. (Honours) Part-III Practical, Medicinal Chemistry,ManikImran Nur Manik
Synthesis of drug & drug intermediates: Paracetamol b) Benzocaine c) Aspirin d) Phenacetin e) PABA (Para amino-benzoic acid f) Meta Nitro-benzaldehyde g) Ethyl para hydroxy-benzoate h) Para Amino phenol i) Methyl salicylate.
1) The document describes the procedure for synthesizing benzimidazole from o-phenylenediamine and formic acid.
2) Key steps include heating a mixture of o-phenylenediamine and excess formic acid at 100°C for 2 hours, then making the reaction mixture alkaline with sodium hydroxide to precipitate crude benzimidazole.
3) Benzimidazole has biological applications as an active component in anthelmintic and antiulcer drugs, and its derivatives also show antimicrobial and anticancer properties.
This document describes the procedure for preparing adipic acid from cyclohexanol via oxidation. Cyclohexanol is oxidized using nitric acid and ammonium metavanadate catalyst at 65-70°C to yield adipic acid crystals. The theoretical and experimental yields and melting point of adipic acid are calculated and measured. Adipic acid is an important industrial dicarboxylic acid used to produce nylon polymers.
This document describes the preparation of p-nitro acetanilide from acetanilide. Acetanilide is nitrated using nitric and sulfuric acid. This produces p-nitro acetanilide as the major product along with a minor amount of o-nitro acetanilide. The p-nitro acetanilide product is purified by recrystallization from ethanol, yielding colorless crystals. Percent yield of the product is calculated and the melting point is obtained and compared to literature values.
This document describes the synthesis of benzanilide from aniline via a Schotten-Baumann reaction. Aniline reacts with benzoyl chloride in the presence of sodium hydroxide to form benzanilide and hydrochloric acid. The reaction involves benzoylation, where the benzoyl group is inserted in place of the active hydrogen on the amine group of aniline. Details of the reaction mechanism, chemicals used, equipment needed and procedure for synthesizing benzanilide are provided. The theoretical and percent yields are also calculated.
Wear gloves and safety goggles. Work in the fume hood.
Procedure:
1. Dissolve benzaldehyde (208 mg, 2 mmol) in ethanol (2 mL) in a test tube.
2. In a separate test tube, dissolve hydroxylamine hydrochloride (189 mg, 2.4 mmol) in ethanol (2 mL).
3. Slowly add the hydroxylamine hydrochloride solution to the benzaldehyde solution with stirring.
4. Add sodium hydroxide pellets (140 mg, 3.5 mmol) and stir until reaction is complete.
5. Extract the product by adding diethyl ether (2 mL) and collecting the ether layer.
This document describes an experiment to synthesize aspirin. Students will learn the process of preparing aspirin through acetylation of salicylic acid with acetic anhydride. They will purify the product and test for the absence of salicylic acid using ferric chloride to form complexes. The history of aspirin's development is outlined from its identification in willow bark to its commercial production. Aspirin's structure and the two-step industrial synthesis from phenol and carbon dioxide is also summarized.
This document discusses different methods of distillation used to purify organic compounds. It describes simple distillation, which involves heating a liquid mixture until it boils and condenses the vapors. Vacuum distillation uses reduced pressure to boil compounds with high boiling points. Steam distillation separates water-immiscible compounds. Fractional distillation employs a fractionating column to separate mixtures with similar boiling points into pure fractions. The document also explains reflex distillation, which prevents evaporation of reactants during a reaction by condensing and returning vapors.
Aspirin is synthesized from salicylic acid using acetic anhydride as a reactant. Salicylic acid is reacted with excess acetic anhydride in the presence of phosphoric acid as a catalyst. Water is then added which causes aspirin to precipitate out of solution. The crude aspirin product is analyzed using melting point determination, titration, and UV-Vis spectroscopy. The purity and percent yield of the aspirin product are calculated from these analytical methods.
Extraction is defined as a process that involves separating active plant or animal components from inactive ones using selective solvents. There are several extraction processes, including infusion, maceration, digestion, decoction, continuous hot extraction, solvent-solvent precipitation, and liquid-liquid extraction. Caffeine is extracted from coffee seeds through infusion by steeping the seeds in water. The caffeine can then be isolated from the tea solution through a multi-step process involving extraction with methylene chloride followed by evaporation of the solvent.
Extraction is defined as a process that involves separating active plant or animal components from inactive ones using selective solvents. There are several extraction processes, including infusion, maceration, digestion, decoction, continuous hot extraction, solvent-solvent precipitation, and liquid-liquid extraction. Caffeine is extracted from coffee seeds through infusion by steeping the seeds in water. It is then isolated from the tea solution through liquid-liquid extraction using methylene chloride followed by evaporation of the solvent to yield caffeine.
This document provides instructions and procedures for 12 organic chemistry laboratory experiments to be conducted by students in an Organic Chemistry Laboratory course. The experiments cover various fundamental organic chemistry techniques including synthesis of aspirin, determination of melting points, distillation, extraction, thin layer chromatography, isolation of natural products, free radical chlorination, SN1 and SN2 reactions, dehydration reactions, Grignard synthesis, computational chemistry, and multiple step synthesis. Detailed procedures are provided for each experiment along with background information on the principles and techniques involved.
The document classifies pharmaceutical products into solids, semi-solids, liquids, and gases and describes common examples of each type such as tablets, creams, syrups, and inhalers. It then discusses the manufacturing process for solid oral dosage forms like tablets and capsules which involves steps like blending, granulation, compression, and coating. Key equipment used includes drying equipment, tablet presses, coating machines, and quality control instruments.
The document describes the process of purifying the organic compound acetanilide through recrystallization. Recrystallization involves dissolving the compound in a heated solvent, then slowly cooling the solution to form pure crystals which can be separated from impurities. Key steps include choosing a solvent where the compound is more soluble when hot than cold, dissolving the compound with minimal heated solvent, adding carbon to remove color, slowly cooling the solution to form crystals, filtering to separate crystals from the remaining solution, and drying the pure crystals. The purity of the purified compound can be assessed by observing its color and measuring its melting point.
This experiment involves a three-step Grignard reaction to synthesize an alcohol from an alkyl halide and acetone. First, the alkyl halide reacts with magnesium metal to form a Grignard reagent. Second, the Grignard reagent reacts with acetone to form an alcohol. Third, the alcohol is recovered by acidifying the reaction mixture. The student purifies the crude alcohol product by fractional distillation and uses chemical tests and IR spectroscopy to analyze the fractions and determine if any side products are present. The objectives are to synthesize an alcohol using the Grignard reaction and characterize any side products that may have formed.
The document provides information about recrystallization, including definitions, types of impurities, and the recrystallization process. It describes recrystallization as a method to purify organic compounds that are solids at room temperature by removing impurities. The key steps involve choosing a solvent based on solubility tests, dissolving the compound in hot solvent, slowly cooling the solution to form crystals of the pure compound, filtering and drying the crystals. Common solvents used in recrystallization are water, ethanol, methanol, hexanes and toluene. Care must be taken to use minimum amounts of hot and cold solvent to avoid losing product. The document also gives procedures for purifying phthalic acid and an unknown
The document discusses various physiochemical processes including precipitation, evaporation, exsiccation, desiccation, and efflorescence. It provides details on precipitation methods such as organic solvent, pH change, and double decomposition. It explains factors that affect evaporation like temperature, surface area, and atmospheric pressure. Exsiccation is the process of removing water of crystallization from hydrated substances by heating. Desiccation completely removes adhered moisture from substances. Efflorescence is the loss of water from hydrated substances into the atmosphere to reach equilibrium between the substance and surroundings.
This document discusses the manufacture of small volume and large volume parenterals. Small volume parenterals have volumes less than or equal to 100ml and are supplied in single or multiple doses, while large volume parenterals have volumes greater than 100ml and are delivered via intravenous route. The key aspects of formulation include therapeutic agents, vehicles like water for injection, and added substances like antimicrobials, antioxidants and buffers. Terminal sterilization is used to assure sterility of the finished products.
This document describes the synthesis of adipic acid from cyclohexanone via a nitric acid oxidation reaction. The reaction is exothermic and the nitric acid must be added slowly to cyclohexanone. Once complete, the product crystallizes and is washed and dried. The percent yield was 62.33% and melting point was 148-151°C, slightly lower than literature due to residual solvent. Infrared spectroscopy confirmed the product was adipic acid. Safety precautions are described for handling oxidizing and acidic reagents.
This document discusses an OSHA compliance report regarding a company called Heritage Thermal Services. According to the report, OSHA cited the company for failing to properly monitor work areas, evaluate respirator effectiveness, implement decontamination procedures, and provide/ensure proper personal protective equipment use. The report indicates an employee was exposed to toxic aniline, which sent them to the hospital. OSHA found the company violated the General Duty Clause by not following mandated safety practices.
This document provides instructions for an experiment to determine the concentration of lead in soil samples using atomic absorption spectroscopy. Students will analyze three related soil samples and develop a hypothesis about the expected trend in lead concentrations between the samples. They will then prepare lead standards, digest the soil samples to extract lead, and use an atomic absorption spectrometer to measure the lead concentration in each sample. The results will be analyzed to compare the expected and measured trends in lead levels across the samples.
This document provides microscale procedures for crystallizing various organic compounds including phthalic acid, naphthalene, and anthracene. It describes dissolving the compounds in solvents like water or alcohols, heating the solutions, adding decolorizing charcoal if needed, cooling to allow crystallization, collecting the crystals through filtration or centrifugation, and calculating percent recovery. Safety instructions are included for proper disposal of solvents and other waste.
Sterile formulations – large and small volume parenterals (1).pptxMamtanaagar1
This document discusses the manufacture of small volume parenterals (SVPs) and large volume parenterals (LVPs). SVPs have volumes less than or equal to 100mL and are used to dispense most drugs, while LVPs have volumes over 100mL and are used to provide electrolytes and nutrition. The document covers formulation aspects like therapeutic agents, vehicles, additives, and containers used. It also discusses production processes like water purification using reverse osmosis or distillation, terminal sterilization, and blow-fill-seal technology. Key differences between SVPs and LVPs are volume, route of administration, use of preservatives and buffers, and isotonicity requirements.
This document provides instructions for synthesizing sulphanilamide from acetanilide in 3 steps:
1. Acetanilide is treated with chlorosulphonic acid to form the intermediate p-acetamidobenzenesulphonyl chloride.
2. p-acetamidobenzenesulphonyl chloride is reacted with ammonia to form p-acetamidobenzenesulphonamide.
3. p-acetamidobenzenesulphonamide undergoes acid hydrolysis with hydrochloric acid to remove the acetamide group and yield the final product sulphanilamide hydrochloride.
The percentage yield of sulphan
Running Head: Lab Report
Lab Report 11
Name: Erricul Harris
Course:
Date:
To demonstrate which part of the fly thorax cell homogenate and carries out glycosis and which part carries out respiration
Table of Contents
2Abstract
2Introduction
2Cell Fractionation
3Methods
3Part A: Preparation of homogenate
6Part B: Biochemical analysis of fractionated homogenate
7Results and Analysis
11Discussion and conclusion
13References
Abstract
This experiment is performed to demonstrate which part of the fly thorax cell homogenate and carries out glycolysis and which part carries out respiration. Flies mainly have three body parts namely the head, thorax and abdomen. The thorax is the part holding the wings and legs. The lab experiment was conducted basing the general knowledge on flies and their body parts. More importantly, it was based on good knowledge of living cells of the flies which is useful in discussing the transportation of glycolysis and carrying out of respiration in the body of a fly. The lab results were then obtained by collecting the flies whose body parts were used to test the assumption that the mitochondrion cells are found in the thorax. Color observations were recorded to determine the usage of oxygen and therefore giving required results. It was observed that glucose was used fast in the test tubes used for the experiment. It was therefore concluded that respiration takes place in the thorax of flies. This experiment is significant in finding out the location of cells used for respiration in flies.
Introduction
Cell Fractionation
There are two major pieces of evidence that give us the details and the process on intercellular booth; (1) evidence obtained from biological and physical separation of intercellular constituents actual (2) inferences obtained through observation by an aid of a microscope from microscopic observation(Keeton, n.d.). The experiment aims at provision of evidence for localization of the cellular respiration of glycolysis and that of mitochondria as cytoplasm soluble; hence, verify the various function of particular cell part. This experiment furthermore aims at a separation of different cell organelles to obtain mitochondria using sophisticated lab research to exploit on the procedure to execute these results. I chose a system that yields a high harvest of mitochondria that are keys our procedure yields an abundant harvest of mitochondria.
In the experiment, I employed two methods on my research: Centrifugation and homogenization. Homogenization produces a solution is which consist of a suspension which is insoluble and soluble cell constituents. The suspension contains intracellular as reference results which have mitochondria organelles(Raven & Johnson, n.d.). Suspension and soluble cell components were separated using centrifugal. The material was spun in a centrifuge ...
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it describes the bony anatomy including the femoral head , acetabulum, labrum . also discusses the capsule , ligaments . muscle that act on the hip joint and the range of motion are outlined. factors affecting hip joint stability and weight transmission through the joint are summarized.
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A Strategic Approach: GenAI in EducationPeter Windle
Artificial Intelligence (AI) technologies such as Generative AI, Image Generators and Large Language Models have had a dramatic impact on teaching, learning and assessment over the past 18 months. The most immediate threat AI posed was to Academic Integrity with Higher Education Institutes (HEIs) focusing their efforts on combating the use of GenAI in assessment. Guidelines were developed for staff and students, policies put in place too. Innovative educators have forged paths in the use of Generative AI for teaching, learning and assessments leading to pockets of transformation springing up across HEIs, often with little or no top-down guidance, support or direction.
This Gasta posits a strategic approach to integrating AI into HEIs to prepare staff, students and the curriculum for an evolving world and workplace. We will highlight the advantages of working with these technologies beyond the realm of teaching, learning and assessment by considering prompt engineering skills, industry impact, curriculum changes, and the need for staff upskilling. In contrast, not engaging strategically with Generative AI poses risks, including falling behind peers, missed opportunities and failing to ensure our graduates remain employable. The rapid evolution of AI technologies necessitates a proactive and strategic approach if we are to remain relevant.
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2. Contents ........ What is Microscale Chemistry ? Why Microscale Chemistry ? Basic Equipment. Synthesis of Aspirin. Synthesis of E –Benzal Synthesis of Azodyes Synthesis of 1-Bromo-3-chloro-5-iodobenzene Separation Of Component Mixture
4. Microscale chemistry is an environmentally safe pollution prevention method of performing chemical processes using small quantities of chemicals with out compromising the quality and standard of chemical applications in education and industry. The best way to succeed in this effort is by eliminating chemical waste at the source. Reduction of chemical use to the minimum level at which experiments can be effectively performed
5. Microscale Chemistry is performed by using: 1-Drastically reduced amounts of chemicals 2-Safe and easy manipulative techniques 3-Miniature labware and high quality skills Microscale Chemistry amounts to a Total Quality Management (TQM) approach to the use of chemicals. Microscale Chemistry is recognized as Small scale Chemistry by the International Union of Pure and Applied Chemistry
11. 3-RECRYSTALLIZATION TUBES: Craig Tube: The Craig tube is used for small-scale recrystallization, which is a method for the purification of small quantities of solid compounds. It has two parts: an outer body, which functions like a vial or test tube; and an inner plunger, which fits partly into the body and rests on a ground-glass surface. The ground-glass joint is not greased, so that liquids can leak through it but solids cannot pass.
12. 4-DISTIALLATION HEADS: Claisen Head Hickman Head Claisen Head or Claisen Adaptor: allows introducing chemical reagents (usually liquids) into a reaction mixture without taking apart the whole apparatus. Hickman Distilling Head: The purpose of a still is to heat a liquid until is passes into the gas (vapor) phase, and then allow the vapor to cool and condense back into the liquid phase, with the condensed liquid trapped in a second container. The Hickman still functions like the air condenser in condensing vapors with the cool glass surface, but the liquid drips down the inside to be trapped in a small circular depression, or collar, in the lower part of the tube.
13. 5-DRYING TUBE: The tube is used to protect the reaction from moisture in the atmosphere while still allowing the passage of air to equalize pressure. To accomplish this the tube is packed with a glass wool plug, a quantity of moisture-absorbing solid (the "drying agent"), and another glass wool plug.
14. The flat, long blade can be used to weigh out solids, stir mixtures, remove "O" rings, scratch glass surfaces to induce crystallization 6-MICRO-SPATULA:
19. BACKGROUND (Cont.) : In commercial aspirin products, a small amount of ASA (300 to 400 mg) is bound together with a starch binder and sometimes caffeine and buffers to make an aspirin tablet. The basic conditions in the small intestine break down the ASA to yield salicylic acid, which is absorbed into the bloodstream. The addition of a buffer reduces the irritation caused by the carboxylic acid group of the aspirin molecule. Aspirin can be produced in a one step chemical process by reacting salicylic acid with acetyl chloride, according to the reaction:
20. Aspirin is a white solid that is almost completely insoluble in water. We will use this physical property of our product to separate it from the final solution. If time allows, we will synthesize methyl salicylate, which is another ester of salicylic acid. It occurs in a wide range of plants and is known as ‘oil of wintergreen’. It is still used in candies and in ointments for joint and muscle pains. Salicylic acid methanol Methyl salicylate (wintergreen). Thin layer chromatography (TLC) is used to separate and identify aspirin.
21.
22. Procedure: 1. Place 150 mg (0.001 mol) of salicylic acid in a 10 mL test tube and add 0.1 mL of pyridine (just sufficient to dissolve it) while the tube rests in a ice-cold water bath. Keep the test tube in a hood while you are doing this. 2. For the next step, be sure that the open end of the tube is not pointing toward you or anybody else. Occasionally the reaction goes quickly and shoots material out of the tube! Add one-tenth milliliter of acetyl chloride (slight excess over 0.001 mol )in one portion to the test tube. Again, keep the mixture in a hood! 3. The mixture becomes viscous at this stage. Let the mixture sit in a beaker of cold water bath for 15 min. – it does not need to be in the hood. While waiting, set up a vacuum filter flask with a Buchner funnel and a piece of filter paper which just fits the bottom of the funnel 4. Now add 5 mL of cold water to the test tube and cap it with a rubber stopper. Shake the mixture. Do this cautiously at first until you are sure that no violent reaction is occurring. The mixture should turn cloudy. Shaking is continued until a white product appears (it may takes several minutes, be patient!)
23. 5. Turn on the water faucet all the way and check to be sure you have good suction. Break the suction by disconnecting the tube from the flask (leave the water running). Pour the mixture into the funnel,trying to get as much of the solid transferred as possible.Connect the hose and apply full suction for at least 30 seconds. Wash the crystals with cold water.Break the suction.Do not just turn off the water; Dry them on the filter paper for about 5 min. Part B- Recrystallization 6. Carefully scrape off most of your crystals into a 50 mL beaker. SAVE THE FILTER PAPER! Add about 3 mL of cold water and place the mixture on a hot plate in a hood. Heat until all of the crystals dissolve (check with the instructor if complete solution does not seem to be happening.) When the crystals are completely dissolved in the hot solution, remove the beaker and allow it to cool. You should see nice crystals of aspirin beginning to form! When the recrystallization is complete, filter again, and dry. SAVE THE FILTER PAPER for the next step! Part C- Oil of Wintergreen 1. Place 1.00 gram of salicylic acid in a test tube. (record the actual mass used) 2. Add 5 ml of methyl alcohol and 3 drops of concentrated sulfuric acid. 3. Heat this mixture in a boiling water bath for 15 min. 4. Note the odor of the liquid in your tube. Procedure (cont’d):
27. Safety Notes: Benzaldehyde is irritant,Hydroxyle amine hydrochloride is corrosive,Sodium hydroxyle pellets is corrosive & hygroscopic,Ethanoyic acid is corrosive,Diethyl ether is flammable & irritant. Procedure: VIAL e’ 0.12 ml water NAOH COOL 1-Benzaldehyde 2-hydroxylamine hydrochloride Stir vigorously Neutralize the mixture by the addition of ethanoic acid extracting with diethyl ether Dry with MgSO4
28. 1-Dissolve NaoH in water(0.12ml ) in 1ml reaction vial containing a spin value allow the solution to cool and add ca. 0.02ml of the benzaldehyde followed by ca. 20mg hydroxylamine hydrochloride . 2-Stopper the flack and stir vigorously, briefly stopping the stirring at 5min interval to add further position of benzaldehyde &hydroxylamine until both reagents have been added completely.The reaction mixture will become warm giving a homogenous solution with almond odor indicating the total consumption of the benzaldehyde. 3-Neutralize the mixture by the addition of ethanoic acid &allow the mixture to cool before extracting with diethyl ether. 4-Separate the organic extracts, dry by passing through a column of MgSo4 into a preweighed reaction vial and remove the solvent then record the yield of the product.
31. Procedure: 1-Put eight drops of aminobenzene in a 10 cm3 beaker and add 30 drops of deionised water followed by 15 drops of concentrated hydrochloric acid. Swirl the beaker and then put it in an ice bath. 2-Weigh 0.15 g of sodium nitrite into another beaker and add 1 cm3 of deionised water. Cool the beaker in the ice bath. Add one spatula of urea (this prevents side reactions occurring). 3-Mix the contents of the two beakers together and keep in the ice bath. 4-Weigh 0.45 g of 2-naphthol into another beaker and add 3 cm3 of sodium hydroxide solution. Swirl to dissolve. 5-Take a piece of cotton cloth 2 x 2 cm2 and, using tweezers, dip it into the 2-naphthol solution. Allow the solution to completely soak the cotton. 6-Dip the cloth completely into the diazonium salt solution. A red dye forms in the fibers, dyeing the cloth.
33. An Improved Deamination of 4-Bromo-2-chloro-6-iodoaniline Reductive deamination step---the final step
34. 1-Under a fume hood, 1.65 mL of a 0.75 M isoamyl nitrite_DMF solution is added to a 10-mL round-bottomed flask containing a magnetic spin vane. 2-A reflux condenser is placed on the flask and the flask is clamped in a sand bath heated to 65◦C. 3-With the isoamyl nitrite solution stirring rapidly, a solution of 4-bromo-2-chloro-6-iodoaniline (0.25g, 0.75 mmol) dissolved in a minimal amount of DMF (2mL) is added dropwise to the reaction solution over a period of 5 min.The evolution of nitrogen gas is immediate and continues until all of the aniline solution is added. 4-After the gas evolution is complete (15 min), the reaction mixture is allowed to cool to room temperature and then carefully transferred to a 25-mL Erlenmeyer flask. 5-15mL of 20% aqueous hydrochloric acid solution is added to the reaction mixture and the product is extracted from the reaction mixture into two, 10-mL portions of ether.The combined organic extract is washed with 15 mL of 10% aqueous hydrochloric acid solution, dried over anhydrous magnesium sulfate, filtered, and concentrated to yield the product as a pale copper-colored solid. 6-The crude product is recrystallized from methanol, using a ratio of 6 mL of methanol per gram of product, to give 1-bromo-3-chloro-5-iodobenzene as long, colorless needles (75–80%, m.p. 85–86 ◦C). Procedure:
36. Liquid-liquid extraction is one of the most used methods for isolating an organic compound from a mixture.This technique is commonly used to isolate and purify products from chemical reactions and is also used to isolate natural products.The process can be categorized into two types of liquid-liquid extraction: -The first type takes advantage of the polarity of compounds and uses water to extract or “wash” an organic mixture by removing highly polar materials, such as inorganic salts, strong acids or bases, etc. -Second, acid and base extraction, takes advantage of chemical properties of compounds. Acid extractions are intended to separate basic compounds from an organic mixture. Organic bases, amines, are converted to their corresponding cationic salts by reacting with acids. These salts are then soluble in water and can be separated from the organic mixture.
37. Base extractions have a concept similar to acid extractions. They are intended to separate acidic compounds from an organic mixture. Organic acids, carboxylic acids, are converted to their corresponding anionic salts by reacting with bases. These anionic salts are usually soluble in water and can be extracted from the organic mixture.
38. Purpose: In this experiment you will be given a three-component mixture, an acid (benzoic acid), a base (ethyl- 4-aminobenzoate) and a neutral organic compound (9-fluorenone). You will have to separate these three compounds individually from the mixture benzoic acid ethyl-4-aminobenzoate 9-fluorenone
39.
40.
41. Procedure (cont’d): 5-Combine the organic layer, dry the organic layer with Na2SO4 [i] [1] and evaporate solvent on the steam bath.3 6-The yellow ether solutions remaining in the vials are recombined into the 5 mL vial. Add 1 mL of pure water, shake its content and then allow the layers to settle. Remove and discard the bottom aqueous layer. 7-Add 1 mL of 3 M NaOH into the 5 mL conical vial that has the yellow ether solution (benzoic acid and 9-fluorenone). 8-Cap and thoroughly shake the vial to allow completion of the reaction and the dissolution of the compounds in their respective solvents. Allow the layers to separate. 9-Carefully transfer the bottom layer to a 3 mL conical vial using a Pasteur pipet.To the 3 mL vial add one ml of diethyl ether.Cap and shake its contents.As before, transfer the lower layer, this time to a 10 mL beaker.By now the contents of the beaker should be very pale or colorless.
42. 10-Add dropwise 6 M HCl to the beaker until the mixture is acidic to pH paper. 11-Transfer the acidic solution into the 5 mL conical vial and extract the aqueous solution three times with 1 mL of diethyl ether each. Combine the diethyl ether layers and dry over Na2SO4. 12-Combine the previous left yellow ether layers into a 5 mL conical vial. Add 1 mL of water, cap and shake its contents. Remove and discard the water layer with a pipette. Dry the organic layer with Na2SO4 and evaporate the ether on the steam bath. Procedure (cont’d):
43. Summary of the procedure: By Na2SO4 In 5 ml vial In beaker using a Hirsch funnel adding 1 mL of deionized water
44. Conclusion: The benefits of microscale are perhaps greatest for biology & biochemistry majors as microscale borrows techniques which are have been standard in biochemistry for years also,converting to microscale is one of the best ways to deal with the problem of chemical wastes in academic labs. The bottom line : Microscale is a cost effective, productive and pollution prevention program.