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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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ix
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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