HRID1245026

反应详情

EQUATION

反应方程式

HRID 1245026 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.70 g (24.9 mmol) of imidazole and 1.88 g (12.5 mmol) of t-butyldimethylsilyl chloride were added to a solution of 1.30 g (8.1 mmol) of (2R,8aS)-2-hydroxy-1,2,3,5,6,7,8,8a-octahydroindolizin-7-one [obtained as described in Preparative Example 2(i)′ above] in 30 ml of dichloromethane and the resulting mixture was stirred for 20 hours at room temperature. At the end of this time, water was added and the reaction mixture was extracted with dichloromethane. The organic extract was washed with water and concentrated by evaporation under reduced pressure, and the resulting residue was then purified by chromatography on an alumina column using a 9:1 by volume mixture of hexane and ethyl acetate as the elaunt to afford 1.98 g (yield: 88%) of the title compound as a colorless oil.

WORKUP

后处理

  1. customobtained
  2. extractionthe reaction mixture was extracted with dichloromethane
  3. extractionThe organic extract
  4. washwas washed with water
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customthe resulting residue was then purified by chromatography on an alumina column
  7. additionby volume mixture of hexane and ethyl acetate as the elaunt