Cyclodextrin experimental procedure

The solution reactions were carried out with or without cyclodextrins in (CH3)2S0, (CH3)2SO-d0 or carbon tetrachloride. The typical experimental procedure was as follows. tra/7S-Cinnamic acid (11 mg, 0.08 mmol), powdered cx-cyclodextrin complex (162 mg, contained 0.08 mmol of the acid), and 3-cyclodextrin complex (100 mg, contained 0.08 mmol of the acid) were dissolved in 0.4 ml of (CH3)2S0-d6, to which 0.1 ml of the same solvent containing bromine (0.08 mmol) was added at 25°C. At 2 h intervals, the conversion of the acid was determined by NMR spectra. Then the reaction mixtures were poured into 20 ml of 15 wt % aqueous sodium chloride soluticn, followed by extraction with diethyl ether. The products were obtained as white solid by evaporation of the ether layer and their optical rotations were measured in ethanol on a polarimeter. 

A typical experimental procedure is as follows The inclusion complex (ca. 2 g or 1 mmol) or ethyl trans-cinnamate with a-cyclodextrin was exposed to gaseous hydrogen bromide (ca. 2 molar ratio) in a desiccator (ca. 600 ml) in the dark under air at 20 C, After exposure of 20 hr, the excess of the gas was removed by evacuation and the complex was dis-... 

The synthetic procedure varies a little with the type of silane reagent that is used and this will depend on the type of linkage that is employed between Ae cyclodextrin and the active group of the silane reagent. In a similar manner, the method of linkage used will also determine the experimental conditions used to bond the cyclodextrin to the silica. An example of the bonding process is depicted below. 

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