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Blackie Academic and Professional, London, 1997

ISBN 0 7514 0225 7

CONTENTS

Preface

Chapter 1.	General  Introduction.

Chapter 2.	Preliminaries.
	2.1	The laboratory
	2.2	The literature
	2.3	Keeping records
	2.4	Safety

Chapter 3.	Bench-Top Techniques.
	3.1	Introduction to inert atmosphere techniques
	3.2	The inert-gas/vacuum double manifold
	3.3	Schlenk techniques
	3.4	Syringe and cannula techniques
	3.5	Apparatus

Chapter 4.	Glove Boxes.
	4.1	Introduction
	4.2	General features
	4.3	Maintenance and use

Chapter 5.	Operations on the high vacuum line.
	5.1	Introduction
	5.2	The high-vacuum line
	5.3	Manipulating volatile materials
	5.4	High-vacuum pumps
	5.5	Alternative designs of high-vacuum lines

Chapter 6.	Solvents and reagents.
	6.1	Introduction
	6.2	Purifying and storing solvents
	6.3	Design and maintenance of solvent stills
	6.4	Reagents
		6.4.1	Halogenation
		6.4.2	Ligand metathesis
		6.4.3	Alkylation
		6.4.4	Reduction
		6.4.5	Oxidation
		6.4.6	Deprotonation
	6.5	Gases

Chapter 7.	Carrying Out Reactions in Solution.
	7.1	Introduction and general considerations
	7.2	Measuring out reagents
	7.3	Transferring solvents
	7.4	Mixing
	7.5	Heating
	7.6	Cooling
	7.7	Monitoring the reaction

Chapter 8.	Reaction Work-Up.
	8.1	Introduction
	8.2	Isolating products
	8.3	Purifying products
	8.4	Storing products

Chapter 9.	Reactions Between a Solid and a Gas.
	9.1	Introduction
	9.2	Designing apparatus
	9.3	Procedure
Chapter 10.           Reactions Between Solids.
	10.1	Introduction
	10.2	General considerations
	10.3	Choice of container
	10.4	Typical procedures

Chapter 11.	Product Identification.
	11.1	Introduction
	11.2	Spectroscopic techniques
		11.2.1	NMR spectroscopy
		11.2.2	Vibrational spectroscopy
		11.2.3	Electronic spectroscopy
	11.3	Mass spectrometry
	11.4	Elemental microanalysis and molecular weight determinations
	11.5	Growing crystals for single-crystal X-ray diffraction
	11.6	Powder X-ray diffraction
	11.7	Other techniques
		11.7.1	Conductivity measurements
		11.7.2	ESR spectroscopy
		11.7.3	Mössbauer spectroscopy
		11.7.4	Thermogravimetry
		11.7.5	Magnetic measurements
		11.7.6	Determination of melting point

Chapter 12.	Special Techniques
	12.1	Introduction
	12.2	Electrochemical techniques
	12.3	Thermal analysis
	12.4	High pressure reactions
	12.5	Photochemical reactions
	12.6	Sonication
	12.7	Microwave heating
	12.8	Reactions in special solvents
	12.9	Matrix isolation
	12.10	Metal vapour synthesis

Chapter 13.	Preparation of Starting Materials
	13.1	Introduction
	13.2	Halides and their simple derivatives
	13.3	Amides
	13.4	Alkoxides and related compounds
	13.5	Oxo compounds
	13.6	Organoimido complexes
	13.7	Carbonyls
	13.8	Cyclopentadienyl complexes
	13.9	Miscellaneous compounds
	13.10	Ligands and reagents

Appendices.
	I	Safety
	II	Deoxygenation columns
	III	Solvents
	IV	NMR solvents
	V	Gases