HRID1659069

反应详情

EQUATION

反应方程式

HRID 1659069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

A solution of β-(2'-chloro-4-biphenylyl)propionyl chloride (28 g.) in anhydrous ether 1 l. is cooled to -70°C. To it is added dropwise a solution of 3M methylmagnesium bromide in ether (34 ml.). The reaction is stirred vigorously throughout. When addition of the grignard is complete (approx. 1 hr), the mixture is allowed to come to room temperature and is decomposed by adding carefully a saturated ammonium chloride solution (approx. 500 ml). The ether phase is washed with brine, dried over sodium sulfate, evaporated in vacuo and the residue distilled to yield 4-(2'-chloro-4-biphenylyl)butan-2-one.

WORKUP

后处理

  1. additionWhen addition of the grignard
  2. custom(approx. 1 hr)
  3. customto come to room temperature
  4. washThe ether phase is washed with brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. distillationthe residue distilled