Supported Reagents: Preparation, Analysis, and Applications Book

1 Introduction to Supported Reagent Chemistry
1.1 Definitions
1.2 The Importance of Supported Reagents
1.3 Choice of Support Material
1.4 Supported Reagents in Organic Synthesis
2 Preparation of Supported Reagents
2.1 Support Pretreatments
2.1.1 Support drying
2.1.2 Hydrolysis of surface groups
2.2 Methods of Preparation
2.2.1 Evaporation
2.2.2 Precipitation
2.2.3 Adsorption from solution
2.2.4 Mixing/grinding
2.2.5 In situ
2.2.6 Ultrasound
2.2.7 Specific syntheses
2.2.8 Substrate adsorption
2.2.9 Ion exchange
2.3 Choice of Loading
2.3.1 Correct loading
2.3.2 Underloading
2.3.3 Overloading
2.4 Choice of Solvent
2.5 Supported Reagent Posttreatment
2.5.1 Further reactions
2.5.2 Thermal posttreatment
3 Analytical Techniques for Studying Supported Reagents
3.1 Introduction
3.2 Infrared Spectroscopy
3.2.1 Direct characterization of surface species
3.2.2 Studies of reagent dispersion
3.2.3 Studies via probe molecules
3.3 Electron Spectroscopy
3.3.1 Ultraviolet--visible spectroscopy
3.3.2 X-Ray Photoelectron and Auger Electron Spectroscopy
3.4 Magnetic Resonance
3.4.1 Nuclear magnetic resonance spectroscopy
3.4.1.1 Direct characterization of surface species
3.4.1.2 Studies of surfaces by probe molecules
3.4.1.3 Other applications of NMR
3.4.2 Electron spin resonance
3.5 Thermal Analysis
3.5.1 Thermogravimetry (TG)
3.5.2 Differential Scanning Calorimetry (DSC)
3.6 X-Ray Techniques
3.6.1 Powder X-ray diffraction
3.6.2 Extended X-ray absorption fine structure (EXAFS)
3.7 Scanning Electron Microscopy
3.8 Mass Spectrometry
3.9 NonspectroscopicMethods
3.9.1 Acid and base strength and site distribution measurements
3.9.2 Measurement of nonacidic or basic sites
3.9.3 Measurement of surface area, pore volume, and pore diameter
4 Case Studies
4.1 Supported Fluorides
4.2 Supported Thiocyanates
4.2.1 KSCN--SiO2
4.2.2 Optimization of reagents
4.2.3 Effect of exposed surface
4.2.4 Allyl and t-alkyl substrates isomerization
4.2.5 CuSCN--charcoal
4.3 Friedel--Crafts Alkylation and Acylation Using Aluminosilicate-based Catalysts
4.3.1 Disadvantages of conventional Friedel--Crafts catalysts
4.3.2 Alkylation
4.3.3 Acylation
Appendix 1
Organic Synthesis Using Supported Reagents
Oxidation and Reduction
Addition to C--Heteroatom Multiple Bonds
Addition to C--C Multiple Bonds
Intramolecular Rearrangement
Aromatic Substitution
Elimination
Aliphatic Substitution
Index