HRID537722

反应详情

EQUATION

反应方程式

HRID 537722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1 g of 17α,21-dihydroxy-pregna-4-ene-3,20-dione and 10 ml of trifluoroethyl butanoate in 50 ml of methyl ethyl ketone was reacted at 45° C. in the presence of 5 g of Candida cylindracea lipase for 8-10 hours, adding at regular time intervals 1 g of lipase. After completion of the reaction, the lipase was filtered off, the filtrate was concentrated under vacuum, taking up the residue three times with solvent. The semi-solid residue was purified by chromatography on a silica gel column with a dichloromethane/methanol 99:1 mixture. The richer fraction was evaporated to obtain 0.89 g (2.14 mM) of 17α-hydroxy-21-butanoyloxy-pregna-4-ene-3,20-dione.

WORKUP

后处理

  1. customwas reacted at 45° C. in the presence of 5 g of Candida cylindracea lipase for 8-10 hours
  2. additionadding at regular time intervals 1 g of lipase
  3. customAfter completion of the reaction
  4. filtrationthe lipase was filtered off
  5. concentrationthe filtrate was concentrated under vacuum
  6. customThe semi-solid residue was purified by chromatography on a silica gel column with a dichloromethane/methanol 99:1 mixture
  7. customThe richer fraction was evaporated