HRID1492605

反应详情

EQUATION

反应方程式

HRID 1492605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Lithium aluminum hydride (9 mL of a 1M solution in THF) was added cautiously to a solution of the product of Step D at 0° C., and the reaction mixture was stirred overnight. Ethyl acetate was added to the mixture, cooled to 0° C. and treated with cold 1N HCl. After separating the organic phase, the aqueous phase was extracted with a mixture of ethyl acetate-ether-dichloromethane. The combined organic extracts were dried and concentrated. The concentrated material was purified by flash column chromatography using 20% ethyl acetate in hexane to afford 4.2 g (92%) of the title compound.

WORKUP

后处理

  1. customAfter separating the organic phase
  2. extractionthe aqueous phase was extracted with a mixture of ethyl acetate-ether-dichloromethane
  3. customThe combined organic extracts were dried
  4. concentrationconcentrated
  5. customThe concentrated material was purified by flash column chromatography