(Ebook) Advanced Practical Organic Chemistry 3rd Edition by John Leonard, B Lygo, Garry Procter ISBN 143986098X 9781439860984

(Ebook) Advanced Practical Organic Chemistry 3rd Edition by John Leonard, B Lygo, Garry Procter ISBN 143986098X 9781439860984

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ISBN 10: 143986098X 
ISBN 13: 9781439860984
Author: John Leonard, B Lygo, Garry Procter

Any research that uses new organic chemicals, or ones that are not commercially available, will at some time require the synthesis of such compounds. Therefore, organic synthesis is important in many areas of both applied and academic research, from chemistry to biology, biochemistry, and materials science. The third edition of a bestseller, Advanced Practical Organic Chemistry is a guide that explains the basic techniques of organic chemistry, presenting the necessary information for readers to carry out widely used modern organic synthesis reactions. This book is written for advanced undergraduate and graduate students as well as industrial organic chemists, particularly those involved in pharmaceutical, agrochemical, and other areas of fine chemical research. It provides the novice or nonspecialist with the often difficult-to-find information on reagent properties needed to perform general techniques. With over 80 years combined experience training and developing organic research chemists in industry and academia, the authors offer sufficient guidance for researchers to perform reactions under conditions that give the highest chance of success, including the appropriate precautions to take and proper experimental protocols. The text also covers the following topics: Record keeping and equipment Solvent purification and reagent preparation Using gases and working with vacuum pumps Purification, including crystallization and distillation Small-scale and large-scale reactions Characterization, including NMR spectra, melting point and boiling point, and microanalysis Efficient ways to find information in the chemical literature With fully updated text and all newly drawn figures, the third edition provides a powerful tool for building the knowledge on the most up-to-date techniques commonly used in organic synthesis.

(Ebook) Advanced Practical Organic Chemistry 3rd Table of contents:

chapter one General introduction
chapter two Safety
2.1 Safety is your primary responsibility
2.2 Safe working practice
2.3 Safety risk assessments
2.4 Common hazards
2.4.1 Injuries caused by use of laboratory equipment and apparatus
2.4.2 Toxicological and other hazards caused by chemical exposure
Table 2.1 Common Hazards with Apparatus in the Chemical Laboratory
2.4.3 Chemical explosion and fire hazards
Table 2.2 Common Chemical Exposure Hazards
Table 2.3 Common Pyrophoric Hazards
Table 2.4 Common Functional Groups with Chemical Explosion Hazards
2.5 Accident and emergency procedures
Bibliography
chapter three Keeping records of laboratory work
3.1 Introduction
3.2 The laboratory notebook
3.2.1 Why keep a laboratory book?
3.2.2 Laboratory records, experimental validity, and intellectual property
3.2.3 How to write a laboratory book: Paper or electronic
Figure 3.1 An example of a laboratory notebook entry.
3.2.4 Paper laboratory notebook: Suggested laboratory notebook format
3.2.5 Electronic laboratory notebooks
3.3 Keeping records of data
3.3.1 Purity, structure determination, and characterization
3.3.2 What types of data should be collected?
3.3.3 Organizing your data records
Figure 3.2 An example of a fixed-format data sheet.
Figure 3.3 A flexible format data sheet (word processor file).
3.4 Some tips on report and thesis preparation
Figure 3.4 A completed data sheet.
3.4.1 Sections of a report or thesis
3.4.2 Planning a report or thesis
3.4.3 Writing the report or thesis
Table 3.1 Suggested Key Phrases for a Standard Experimental Method
Figure 3.5 Tabulated experimental data for inclusion in a thesis.
Figure 3.6 An example of a journal-specific experimental procedure.
Bibliography
chapter four Equipping the laboratory and the bench
4.1 Introduction
4.2 Setting up the laboratory
4.3 General laboratory equipment
4.3.1 Rotary evaporators
4.3.2 Refrigerator and/or freezer
4.3.3 Glass-drying ovens
4.3.4 Vacuum oven
4.3.5 Balances
4.3.6 Kugelrohr bulb-to-bulb distillation apparatus
4.3.7 Vacuum pumps
Figure 4.1 Single manifold.
4.3.8 Inert gases
4.3.9 Solvent stills
4.3.10 General distillation equipment
Figure 4.2 One-piece distillation apparatus.
Figure 4.3 One-piece distillation apparatus incorporating a fractionating column.
4.3.11 Large laboratory glassware
4.3.12 Reaction monitoring
4.4 The individual bench
4.4.1 Routine glassware
Table 4.1 A Typical Set of Routine Glassware for Synthetic Organic Chemistry
Table 4.2 Standard, Commercially Available Items That Should Be Included in an Individual Bench Kit
4.4.2 Additional personal items
4.4.3 Specialized personal items
4.4.3.1 Double manifold
Figure 4.4 Double manifold.
Figure 4.5 Cross section of a double-oblique tap: (a) tap switched to vacuum and (b) tap switched to inert gas.
Figure 4.6 A simple bubbler design.
Figure 4.7 Double manifold connected to a vacuum line and an inert gas supply.
Figure 4.8 Spaghetti tubing manifold.
4.4.3.2 Three-way Quickfit gas inlet T taps
Figure 4.9 Three-way taps.
Figure 4.10 Using a three-way tap.
4.4.3.3 Filtration aids
Figure 4.11 One-piece sintered filter funnels.
Figure 4.12 Small-scale recrystallization apparatus: (a) one-piece filtration apparatus and (b) Craig tube.
4.4.3.4 Glassware for chromatography
Figure 4.13 Inert atmosphere filtration apparatus.
Figure 4.14 Flash chromatography column: (a) flash adapter, (b) flash valve, (c) flash column, and (d) reservoir.
4.5 Equipment for parallel experiments
4.5.1 Simple reactor blocks that attach to magnetic stirrer hot plates
4.5.2 Stand-alone reaction tube blocks
4.5.3 Automated weighing systems
4.5.4 Automated parallel dosing and sampling systems
4.6 Equipment for controlled experimentation
4.6.1 Jacketed vessels
Figure 4.15 Jacketed vessel and lid.
Figure 4.16 A syringe pump.
4.6.2 Circulating heater-chillers
4.6.3 Peltier heater-chillers
4.6.4 Syringe pumps
4.6.5 Automated reaction control systems
4.6.6 All-in-one controlled reactor and calorimeter systems
chapter five Purification and drying of solvents
5.1 Introduction
5.2 Purification of solvents
5.3 Drying agents
5.3.1 Alumina, Al2O3
5.3.2 Barium oxide, BaO
5.3.3 Boric anhydride, B2O3
5.3.4 Calcium chloride, CaCl2
5.3.5 Calcium hydride, CaH2
5.3.6 Calcium sulfate, CaSO4
5.3.7 Lithium aluminum hydride, LiAlH4
5.3.8 Magnesium, Mg
5.3.9 Magnesium sulfate, MgSO4
5.3.10 Molecular sieves
5.3.11 Phosphorus pentoxide, P2O5
5.3.12 Potassium hydroxide, KOH
5.3.13 Sodium, Na
5.3.14 Sodium sulfate, Na2SO4
5.4 Drying of solvents
5.4.1 Solvent drying towers
Figure 5.1 Solvent drying towers.
5.4.2 Solvent stills
Figure 5.2 A continuous solvent still.
Figure 5.3 Design of how to construct a continous solvent still collecting head.
5.4.3 Procedures for purifying and drying common solvents
Figure 5.4 Alternative designs for solvent still collecting heads.
5.4.4 Karl Fisher analysis of water content
References
chapter six Reagents: Preparation, purification, and handling
6.1 Introduction
6.2 Classification of reagents for handling
6.3 Techniques for obtaining pure and dry reagents
6.3.1 Purification and drying of liquids
Table 6.1 Examples of Reagents That Should Be Distilled under an Inert Atmosphere
Table 6.2 Examples of Reagents That Can Be Distilled under Reduced Pressure
Table 6.3 Examples of Reagents That Can Be Distilled from Quinoline
6.3.2 Purifying and drying solid reagents
6.4 Techniques for handling and measuring reagents
6.4.1 Storing liquid reagents or solvents under an inert atmosphere
Figure 6.1 Preparing a vessel for storage of air- or moisture-sensitive reagents: (a) flush the container with inert gas, (b) wire on a septum, and (c) use an “inverted” second septum as a seal.
6.4.2 Bulk transfer of a liquid under inert atmosphere (cannulation)
Figure 6.2 Setting up a system for bulk transfer of a liquid under inert atmosphere: (a) apply a positive pressure of inert gas and (b) flush the cannula with inert gas.
Figure 6.3 Bulk transfer of a liquid under inert atmosphere.
6.4.3 Using cannulation techniques to transfer measured volumes of liquid under inert atmosphere
Figure 6.4 Measuring large volumes of liquid under inert atmosphere using either (a) a measuring cylinder or (b) a Schlenk tube.
Figure 6.5 Bulk transfer of measured volumes of liquid under inert atmosphere.
Figure 6.6 Different types of cannula: (a) a standard cannula, (b) a cannula made from two syringe needles and Luer locks, and (c) a “flex-needle.”
Figure 6.7 Making an all-PTFE cannula.
6.4.4 Use of syringes for the transfer of reagents or solvents
Figure 6.8 Liquid-tight syringe.
Figure 6.9 Gas-tight microsyringe.
Figure 6.10 All-glass Luer syringes.
Figure 6.11 Gas-tight Luer syringe.
Figure 6.12 Luer syringe fittings.
Figure 6.13 Luer fitting syringe needles.
Figure 6.14 Flushing a syringe with inert gas.
Figure 6.15 Transferring an air- or moisture-sensitive liquid by syringe: (a) fill the syringe with inert gas, (b) force excess reagent and gas bubbles back into the bottle, and (c) deliver measured volume of reagent.
Figure 6.16 Maintaining inert atmosphere around a syringe needle tip: (a) inert capsule used to protect the tip of the syringe, (b) transfer of the reagent to the syringe with inert capsule in place, (c) pull the tip of the needle into the inert capsule, and (d) deliver the reagent.
6.4.5 Handling and weighing solids under inert atmosphere
Figure 6.17 Weighing a moisture-sensitive metal. (a) Clean metal cut, (b) wash, and (c) wash into beaker of oil and then rewash.
Figure 6.18 Removing oil from a metal dispersion (small-scale): (a) connect to manifold, (b) wash with petroleum ether, and (c) remove the petroleum ether.
Figure 6.19 Removing oil from a metal dispersion (large-scale): (a) place under a positive pressure of inert gas, (b) add petroleum ether, and (c) force petroleum ether through the dispersion.
Figure 6.20 Using an inverted filter funnel to provide an argon blanket.
6.5 Preparation and titration of simple organometallic reagents and lithium amide bases
6.5.1 General considerations
Figure 6.21 Two apparatus setups for the preparation of organometallics: using (a) a mechanical stirrer and (b) an ultrasonic bath.
Figure 6.22 Formation of a Grignard reagent.
6.5.2 Preparation of Grignard reagents (e.g., phenylmagnesium bromide)
6.5.3 Titration of Grignard reagents
6.5.4 Preparation of organolithium reagents (e.g., n-butyllithium)
Figure 6.23 Formation of an organolithium reagent.
6.5.5 Titration of organolithium reagents (e.g., n-butyllithium)
Figure 6.24 Titration of an organolithium reagent.
6.5.6 Preparation of lithium amide bases (e.g., lithium diisopropylamide)
Figure 6.25 Preparation of LDA.
6.6 Preparation of diazomethane
6.6.1 Safety measures
6.6.2 Preparation of diazomethane (a dilute ethereal solution)
Figure 6.26 Apparatus for preparing diazomethane solution.
6.6.3 General procedure for esterification of carboxylic acids
6.6.4 Titration of diazomethane solutions
References
chapter seven Gases
7.1 Introduction
7.2 Use of gas cylinders
Figure 7.1 Gas cylinder head unit.
7.2.1 Fitting and using a pressure regulator on a gas cylinder
Figure 7.2 Gas cylinder regulator plus three-way needle valve outlet.
7.3 Handling gases
Figure 7.3 Typical arrangement for the addition of a gas to a reaction flask.
7.4 Measurement of gases
7.4.1 Measurement of a gas using a standardized solution
Figure 7.4 Setup for dispensing gases via a gas-tight syringe.
7.4.2 Measurement of a gas using a gas-tight syringe
7.4.3 Measurement of a gas using a gas burette
Figure 7.5 Gas burette setup.
7.4.4 Quantitative analysis of hydride solutions using a gas burette
7.4.5 Measurement of a gas by condensation
7.4.6 Measurement of a gas using a quantitative reaction
Figure 7.6 Measurement of a gas by condensation.
7.5 Inert gases
7.6 Reagent gases
Figure 7.7 Gas generator setup.
7.6.1 Gas scrubbers
7.6.2 Methods for preparing some commonly used gases
Figure 7.8 Gas scrubber setup.
References
chapter eight Vacuum pumps
8.1 Introduction
8.2 House vacuum systems (low vacuum)
8.3 Medium vacuum pumps
8.3.1 Water aspirators
Figure 8.1 Water trap for use with water aspirators.
8.3.2 Electric diaphragm pumps
8.4 High vacuum pumps
8.4.1 Rotary oil pumps
Figure 8.2 Cold-finger condenser solvent trap setup for high vacuum pumps.
8.4.2 Vapor diffusion pumps
8.5 Pressure measurement and regulation
Figure 8.3 Figure showing (a) a mercury manometer and (b) a McLeod gauge.
8.5.1 Units of pressure (vacuum) measurement
chapter nine Carrying out the reaction
9.1 Introduction
9.2 Reactions with air-sensitive reagents
9.2.1 Introduction
9.2.2 Preparing to carry out a reaction under inert conditions
9.2.3 Drying and assembling glassware
Figure 9.1 Reaction flask attached to a double manifold.
9.2.4 Typical reaction setups using a double manifold
9.2.5 Basic procedure for inert atmosphere reactions
Figure 9.2 Flow through a three-way tap relative to tap position inert gas flows: (a) only into flask, (b) into flask and to atmosphere, and (c) no inert gas flow.
Figure 9.3 Adding air- or moisture-sensitive liquids to a reaction flask: (a) fill syringe, (b) add solvent from syringe, and (c) turn three-way tap to position A (Figure 9.2).
9.2.6 Modifications to basic procedure
Figure 9.4 Typical setups for inert atmosphere reactions that are to be heated: (a) no septum needed, and (b) septum needed to allow additions via syringe.
Figure 9.5 Larger-scale apparatus for inert atmosphere reactions.
Figure 9.6 Setting up larger-scale apparatus for inert atmosphere reactions. (a) Cooling apparatus under a flow of inert gas. (b) Filling dropping funnel using cannula.
Figure 9.7 Using a double manifold.
Figure 9.8 Transferring liquids via cannula: (a) directly to the reaction flask, and (b) to an addition funnel.
Figure 9.9 Using a solid addition tube: (a) before addition of solid to the reaction, and (b) addition of the solid.
9.2.7 Use of balloons for holding an inert atmosphere
Figure 9.10 Using a balloon to maintain an inert atmosphere: (a) attached via three-way tap to permit evacuation/filling cycles, and (b) attached via a needle and septum.
Figure 9.11 Using a balloon to flush a flask with inert gas.
Figure 9.12 Attaching a balloon to a needle or three-way tap.
Figure 9.13 Using a spaghetti tube manifold.
9.2.8 Use of a “spaghetti” tubing manifold
9.3 Reaction monitoring
9.3.1 Thin layer chromatography
Figure 9.14 Taking a TLC sample from a reaction under inert atmosphere.
Figure 9.15 Running a TLC: (a) spot the plate, (b) run the TLC, and (c) remove and develop the plate.
Table 9.1 TLC Stains
Table 9.2 Recipes for TLC Stains
Figure 9.16 Running a two-dimensional TLC: (a) place spot in one corner, (b) elute plate, and (c) turn plate by 180° and elute again.
9.3.2 High performance liquid chromatography
Figure 9.17 A typical analytical HPLC setup.
Figure 9.18 Schematic of the injection port in load (a) and inject (b) positions.
9.3.3 Gas–liquid chromatography (GC, GLC, VPC)
Figure 9.19 A typical GC setup.
Figure 9.20 Organolithium addition.
9.3.4 NMR
9.4 Reactions at other than room temperature
9.4.1 Low-temperature reactions
Figure 9.21 Using a cooling bath.
Figure 9.22 Monitoring internal temperature using a digital thermometer.
Table 9.3 Ice-Based Cold Baths1
Table 9.4 Dry Ice Cold Baths2
9.4.2 Reactions above room temperature
Table 9.5 Liquid Nitrogen Slush Baths3
Figure 9.23 A simple sealed tube (Carius tube).
Figure 9.24 A reaction tube.
Figure 9.25 A typical setup for performing a reaction at reflux.
Figure 9.26 Different types of condensers: (a) coil condenser, (b) Liebig condenser, (c) double-jacketed condenser, and (d) cold-finger condenser.
Figure 9.27 Using an aluminum heating block.
Figure 9.28 Using a heating mantle.
9.5 Driving equilibria
9.5.1 Dean–Stark traps
Figure 9.29 Using a Dean–Stark trap.
9.5.2 High-pressure reactions
9.6 Agitation
9.6.1 Magnetic stirring
Figure 9.30 Magnetic stirrer machines.
Figure 9.31 Magnetic followers: (a) bar, (b) octagonal, and (c) egg-shaped.
9.6.2 Mechanical stirrers
Figure 9.32 Using a mechanical stirrer.
Figure 9.33 Attaching a PTFE paddle.
Figure 9.34 Apparatus for attaching a stirrer rod to a reaction flask: (a) PTFE joint and (b) ground-glass joint.
9.6.3 Mechanical shakers and vortexers
Figure 9.35 Mechanical shaker.
9.6.4 Sonication
Figure 9.36 Performing a reaction in an ultrasonic cleaning bath.
Figure 9.37 Using an ultrasonic probe.
9.7 Use of controlled reactor systems
9.7.1 Jacketed vessels
9.7.2 Parallel reactors
References

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