反应详情

A mixture of 50% NaOH (10 ml), epichlorohydrin (6 ml) and tetrabutylammonium hydrogen sulfate (0.3 g) kept at 0° C. was added drop by drop to a solution of (3α,5β,7α,12α)-3,7,12-trihydroxy-cholan-24-oic acid 1,1-dimethylethyl ester (prepared according to the procedure described by R. P. Bonar-Law et al., J. Chem. Soc. Perkin Trans. I, 1990, 2245) (0.0045 mol) in CH2Cl2 (10 ml). When the addition was completed the mixture was left to react at room temperature by 24 h. The organic phase was separated, washed with H2O to neutral, dried over Na2SO4 and evaporated. The residue was purified by flash chromatography to obtain 0.86 g of desired product (0.0017 mol).

1. customkept at 0° C.
2. customprepared
3. additionWhen the addition
4. waitwas left
5. customto react at room temperature by 24 h
6. customThe organic phase was separated
7. washwashed with H2O to neutral,
8. dry with materialdried over Na2SO4
9. customevaporated
10. customThe residue was purified by flash chromatography