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Handbook of Practical Pharmaceutical

Organic, Inorganic and Medicinal Chemistry

Handbook of Practical Pharmaceutical Chemistry

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Handbook of Practical

Pharmaceutical Organic, Inorganic

and Medicinal Chemistry

Handbook of Practical Pharmaceutical Chemistry (As per Pharmacy Council of India-B. Pharm and Pharm. D

Syllabus)

Dr. Prasenjit Mondal,

Dr. Sumanta Mondal

EDUCREATION PUBLISHING (Since 2011)

www.educreation.in

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Dedicated

To

Our Parents and Family

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About the authors

Dr. Prasenjit Mondal

Dr. Prasenjit Mondal is an Associate Professor at the Department

of Pharmacy, Sri Vaageswari educational society, Karimnagar,

India. He holds a doctorate in Pharmaceutical science and his

research work focused on the Bioanalytical method development

and validation in human plasma using LC-MS/MS and

pharmacokinetic study. He is an active reviewer of several

Thomson Reuters indexed reputed national and international

journals.

Dr. Prasenjit Mondal is a life member of APTI. He has published

more than 35 research articles in various high impact international

and national journals. He guided more than 25 M.Pharm students.

WHO (World Health Organization) has selected and included the

two analytical methods developed by Dr. Prasenjit Mondal et.al for

the establishment of their official monograph of non-

Pharmacopoeial drug (ETIZOLAM). These standardized methods

recognized by WHO in their expert committee review meeting,

November 2015 at Geneva, Switzerland.

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Dr. Sumanta Mondal

Dr. Sumanta Mondal: Assistant Professor & NSS Programme

Officer of GITAM Institute of Pharmacy, GITAM (Deemed to be

University), Andhra Pradesh, India. His research involves

bioactivity and phytochemical studies of various medicinal plant

species. He has published more than 68 research articles in various

international and national journals. He has guided more than 22 M.

Pharm students and presently seven students are pursuing PhD

under his guidance. He is an active reviewer of several Thomson

Reuters indexed reputed national and international journals

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Preface

The first edition of handbook of practical organic, inorganic and

medicinal chemistry intended to provide the basic guidance of

handling of chemicals, various safety guidelines to be strictly

maintain in chemistry laboratory. It also provides important

laboratory techniques to be used during synthesis of drugs and

chemicals. It gives concise coverage of range of chemical

compounds synthesis procedure as per the Pharmacy council of

India syllabus and more. This book elaborately described about the

concept and procedure involved in the limit test of inorganic

impurities, preparation of various inorganic compounds and salt

analysis. We have incorporated various steps in detail to be

followed for the identification of unknown chemical compounds.

We elaborately explained and methods for the determination of

various analytical constants of fats and oil.

Preparation of various organic compounds and intermediates has

been included as per the B. Pharmacy syllabus. Reactions of every

preparations with detail mechanism has been explained, which will

help the students to understand and can further improve their

practical skills. As per the medicinal chemistry syllabus we

described the procedure for the preparation of useful drugs, the

reaction mechanism involve the synthesis and calculation. The

incorporated methods utilise easily available, economic chemicals

and glass apparatus. The assay methods of various drugs also

included as per the syllabi. At the last chapter we incorporated the

preparations of useful solutions and reagents, that will be require

for the synthesis and assay if mentioned drugs and organic

compounds.

We shall welcome the constructive criticism and suggestions with

a view to improve the present effort.

We are grateful to Prof (Dr) G.K Dash, [Professor and Head

(Research and Post Graduate Studies), University of Kuala

Lumpur, Malaysia], Dr. Arnab Samanta, (Professor & Principal,

Netaji Subhas Chandra Bose Institute of Pharmacy, Chakdaha Dist.

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Nadia, West Bengal) Dr. Satla Sobha Rani, (HOD, Centre for

pharmaceutical science, JNTU Hyderabad) and Dr. R.

Ramakrishna (Vaageswari Institute of Pharmaceutical sciences,

Karimnagar) for their valuable suggestions and blessings. Authors

are also extending their thanks to the Principal & chairman Dr. G

Srineevas Reddy, (Vaageswari Educational Society) and

Prof (Dr) S. Ganapaty, Principal, (GITAM Institute of Pharmacy)

for their constant encouragement.

Finally we owe the sense of gratitude to our parents and family.

There will be always some scope for the further development,

therefore we request all the readers of this book to send their

valuable suggestions for the further additions of valuable contents

to this book.

Dr. Prasenjit Mondal

Dr. Sumanta Mondal

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Contents

Sr. Chapter Page

1. Introduction. 1

2. Laboratory safety guidelines and regulations. 3

3. Various laboratory techniques. 9

3.1. Filtration methods 9

3.2. Steam distillation 14

3.3. Recrystallization 15

4. Limit tests 20

4.1. Chloride 20

4.2. Sulphate 22

4.3. Iron 24

4.4. Lead 26

4.5. Arsenic 30

5. Preparations of various inorganic compounds 33

5.1. Potassium Alum 33

5.2. Magnesium sulphate 35

5.3. Zinc stearate 37

5.4. Copper sulphate 39

5.5. Ferrous Sulpahte 41

5.6. Boric acid 43

5.7. Test for purity of potash alum. 45

5.8. Swelling behaviour of Bentonite 46

5.9. Acid neutralizing capacity aluminium

hydroxide gel.

47

5.10. Determination of iodine and potassium

iodate in potassium iodide.

48

6. Salt analysis 50

6.1. Simple salt analysis-I (Sodium chloride) 78

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6.2. Simple salt analysis-II (Calcium chloride) 80

6.3. Simple salt analysis-III (sodium acetate) 83

6.4. Simple salt analysis-IV (Ammonium

sulphate)

86

6.5. Simple salt analysis-V (Barium sulphate) 89

6.6. Identification test of Magnesium hydroxide. 92

6.7. Identification test of Ferrous sulphate. 94

6.8. Identification test of Sodium bicarbonate. 96

6.9. Identification test of Copper sulphate. 98

6.10. Identification test of Calcium gluconate. 100

7. Melting and boiling points of the organic

compounds

102

8. Identification of unknown compounds 108

8.1. Preliminary examination 108

8.2. Solubility test 110

8.3. Detection of extra elements 112

8.4. Test for unsaturation 115

8.5. Test for alcoholic group 117

8.6. Test for phenolic group 120

8.7. Test for aldehyde and ketones groups 123

8.8. Test for carboxylic group 127

8.9. Test for amino group 129

9. Determination of oil values 131

9.1. Acid value 131

9.2. Saponification value 133

9.3. Iodine value. 136

9.4. Ester value 138

9.5. Acetyl value 139

10. Preparation of organic compounds 141

10.1. Preparation of 5- nitrosalicylic acid. 141

10.2. Preparation of Nitrobenzene 144

10.3. Preparation of Acetanilide 147

10.4. Preparation of p-bromo aniline 149

10.5. Preparation of Dibenzyl acetone 151

10.6. Preparation of 1- phenyl azo 2 naphthol 154

10.7. Preparation of Benzil 156

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10.8. Preparation of Benzanilide 158

10.9. Preparation of Phenyl benzoate 160

10.10. Preparation of Methyl salicylate 163

10.11. Preparation of Cinnamic acid 166

10.12. Preparation of 2,4,6 tribromo aniline 169

10.13. Preparation of Benzoic acid from benzyl

acloride

171

10.14. Preparation of Benzoic acid from alkyl

benzoate.

173

11. Preparation of drugs and intermediates 175

11.1. Preparation of Benzimidazole 175

11.2. Preparation of Benztriazole 178

11.3. Preparation of 2,3- diphenyl quinoxaline 181

11.4. Preparation of Benzocaine 184

11.5. Preparation of Phenytoin 187

11.6. Preparation of Phenothiazine 190

11.7. Preparation of Barbiturate 197

11.8. Preparation of Sulphanilamide 195

11.9. Preparation of 7-Hydroxy 4 methyl

coumarine

201

11.10. Preparation of Chlorobutanol 205

11.11. Preparation of triphenyl imidazole 207

11.12. Preparation of Hexamine 209

12. Assay of drugs 211

211

12.1. Assay of Isonicotinic acid hydrazide 213

12.2. Assay of Aspirin 216

12.3. Assay of Metronidazole. 218

12.4. Assay of Ibuprofen 220

12.5. Assay of chloropheneramine maleate 222

12.6. Assay of furosemide. 224

12.7. Assay of chloropromazine 226

12.8. Assay of Chloroquine phosphate 229

13. Preparation of reagents. 230

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1. Introduction

Chemistry is the basic science of the structure, composition,

properties and reactions, within the atomic and molecular systems.

Life is the full of chemistry; from the composition of the unit of

life, the cell to the whole organism, the presence of chemistry is

conspicuous. Human beings physically are constructed of

chemicals, live in a overabundance of chemicals and are entirely

dependent on chemicals for their quality of modern life. All living

organisms are building of numerous organic substances. Evolution

of life begins from one single organic compound called a

nucleotide. Which join together to form the building blocks of life.

In our everyday life, whatever we see, consume is the gift of

research in chemistry for thousands of years. In fact, chemistry is

applied everywhere in modern life.

The normal daily life of us starts from wakeup and ends with

fall asleep to wake up in the next morning. The entire activity what

we do, things we use, things we eat, entirely related to chemical

compounds, may be synthesized chemical compounds, natural

chemical substances or marine chemical substances. In one

sentence, we are made up off, surrounded by, and cannot live

without the help of a chemical.

It has played a major role in pharmaceutical advances,

forensic science and modern agriculture. Diseases and their

remedies have also been a part of human lives. Chemistry also

plays an immense role in the understanding of diseases and their

remedies, i.e. the discovery and development of drugs.

The development of practical skill, specifically in chemistry

lab can be possible by interacting with abandoned environment of

the material world in laboratory experiences may help students

concretely understand the inherent ambiguity and complexity of

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natural phenomena. Laboratory experiences definitely help the

students to learn and address the challenges inherent in directly

observing and manipulating the material world, including

troubleshooting equipment used to make observations,

understanding measurement error, and interpreting and aggregating

the resulting data. Chemistry experiments is the science of

observation, here we pose a question to nature, carry out the

corresponding experiment, and observe the result. What happens

when we mix two substances? If we blast a molecule with a laser

beam, what will it do? Experiments produce the data that relate to

each individual observation. On the other hand, theory is

concerned with building general frameworks for placing large

numbers of individual observations into a rational order. It does so

by building mathematical models, deducing general laws, and

using these to predict the outcomes of future experiments. The

tools of theory are usually physics and mathematics applied to

chemical problems. Without theory, experimental science is just a

vast catalogue of irrationalized observations. Without experiment,

theory is simply a long list of speculation with no verification or

falsification.

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2. Laboratory Safety Guidelines

Safety and personnel health considerations are as prime important

as any other thing taught in science curricula. Occupational injury

data from industry studies indicate that the injury rate is highest

during the initial period of employment and decreases with

experience. Similarly, in a chemistry laboratory setting where stu-

dents experience new activities, the chances of incidents, injury,

and damage is high. Therefore, it is essential that the students are

taught what can go wrong, how to prevent such events from

occurring, and what to do in case of an emergency. Therefore the

responsibility of teachers to

• Educate the students on the location and use of entire safety

and emergency equipment before laboratory activity.

• Identify the safety procedures to follow in the event of an

emergency/accident.

• Provide the students with verbal as well as written safety

procedures to avoid the event of an emergency/accident.

• Know the area of and procedure to use the cut-off switches

and valves for the water, gas, and electricity in the

laboratory.

• Know the location of and how to use all safety and

emergency equipment (i.e., eyewash, fire blanket, first-aid

kit, fire extinguishers, safety shower and mercury spill

kits).

• Trained the students by conducting safety and evacuation

drills on a regular basis.

• Explain in detail to students the consequences of violating

safety rules and procedures.

• Keep a list of emergency phone numbers near the phone.

The responsibility also extended to maintenance of chemicals and

preparation of various laboratory activities, described as follows.

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