HRID22997

反应详情

EQUATION

反应方程式

HRID 22997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

46.00 g (140.0 mmol) of the compound obtained in Example 13 (a) and 500 ml of THF are introduced into a three-necked flask under a stream of nitrogen. 61.5 ml (154.00 mmol) of an n-butyllithium solution (2.5M in hexane) are added dropwise at −78° C. and the mixture is stirred for 30 minutes at this same temperature. 13.0 ml (168.0 mmol) of DMF are then added dropwise and the mixture is allowed to return to room temperature. The reaction mixture is acidified with hydrochloric acid (1N) and extracted with ethyl ether and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. 46.00 g (100%) of the expected compound are collected in the form of an orange oil.

WORKUP

后处理

  1. customto return to room temperature
  2. extractionextracted with ethyl ether
  3. customthe organic phase is separated
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. custom46.00 g (100%) of the expected compound are collected in the form of an orange oil