作者: J. T. Sharp , I. Gosney , A. G. Rowley
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摘要: 1 Introduction.- 1.1 The range of experimental techniques.- 1.2 Good laboratory practice.- 1.3 Safety in the laboratory.- 1.3.1 Chemical hazards.- 1.3.2 Fire hazard.- 1.3.3 Vacuum and pressure work.- 1.4 Keeping records.- 1.4.1 Recording data.- 1.4.2 Final reports.- 1.5 Samples spectra.- 2 Carrying out reactions.- 2.1 Basic 2.1.1 Apparatus.- 2.1.2 Addition reactants.- 2.1.3 Stirring reaction mixtures.- 2.1.4 Temperature control.- 2.1.5 Reactions under anhydrous conditions inert atmospheres.- 2.2 Special 2.2.1 use air-and water-sensitive reagents.- 2.2.2 liquid ammonia.- 2.2.3 Catalytic hydrogenation.- 2.2.4 Photochemistry.- 2.2.5 Flash vacuum pyrolysis.- 3 Isolation purification products.- 3.1 Primary work-up procedures.- 3.1.1 General considerations.- 3.1.2 Removal solvent by rotary evaporator.- 3.1.3 Extraction 3.1.4 Drying organic solutions.- 3.1.5 Separation target product(s).- 3.2 Crystallization.- 3.2.1 principles.- 3.2.2 Melting point as a criterion purity.- 3.2.3 Methods crystallization.- 3.2.4 Choosing crystallization solvent.- 3.2.5 topics.- 3.3 point.- 3.3.1 3.3.2 Determination melting 3.3.3 Other methods.- 3.4 Distillation.- 3.4.1 3.4.2 Simple distillation.- 3.4.3 Fractional 3.4.4 Small-scale 3.4.5 Molecular 3.4.6 Steam 3.4.7 Sublimation solids.- 3.4.8 Appendices.- 4 mixtures chromatography.- 4.1 Analytical 4.1.1 Thin-layer description.- TLC plates adsorbents.- Application sample.- Running (developing) chromatogram.- Examining for qualitative analysis.- developing 4.1.2 Gas-liquid instrument.- Injecting Identification GLC.- Quantitative GLC Selection stationary phase other operating parameters.- Setting up instrument, some general points.- 4.1.3 High-performance Equipment.- Operation equipment.- Qualitative quantitative Retention resolution - basics.- Optimizing separation.- chromatographic mode.- Liquid solid (adsorption) chromatography (LSC).- (LLC) on bonded phases.- 4.2 Preparative 4.2.1 thin-layer 4.2.2 Column method.- Dry-column flash Medium-pressure Gravity-elution 4.3 4.3.1 principles 4.3.2 Control adsorbent activity.- 4.3.3 Preparation plates.- samples spectroscopy.- 5.1 Infra-red.- 5.2 Nuclear magnetic resonance.- 5.3 Mass spectrometry.- 5.4 Ultraviolet.- Finding chemical information.- 6.1 Physical properties.- 6.2 Spectroscopic 6.3 Beilstein's Handbuch.- 6.4 Abstracts.