HRID343902

反应详情

EQUATION

反应方程式

HRID 343902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of sodium borohydride (2.0 g) and 40% w/v aqu. NaOH was added dropwise to a solution of the the product from step (b) (1.9 g) in acetonitrile (55 ml) at 0° C. The pH was maintained at 3-6 by periodic additions of 2N aqu. HCl. The resulting solution was stirred at 0° C. for 2 hours, then diluted with water and extracted with DCM. The combined extracts were washed with brine, dried and evaporated in vacuo to give a yellow oil which was eluted through a silica column using chloroform as eluant to give the desired product as a pale yellow oil (0.78 g).

WORKUP

后处理

  1. temperatureThe pH was maintained at 3-6 by periodic additions of 2N aqu
  2. extractionextracted with DCM
  3. washThe combined extracts were washed with brine
  4. customdried
  5. customevaporated in vacuo
  6. customto give a yellow oil which
  7. washwas eluted through a silica column