HRID566545

反应详情

EQUATION

反应方程式

HRID 566545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of ethyl magnesium bromide in diethyl ether (58 ml, 3 M) was added dropwise at room temperature to a mixture of 3-methoxybenzonitrile (21.2 g, 0.159 mol) and dry THF (250 ml). When addition was complete the mixture was stirred for 1 h at room temperature, 3 h at 40° C. and finally stirred overnight at room temperature. Water (250 ml) was added followed by a saturated ammonium chloride solution (250 ml) and the mixture was stirred for 1 h at room temperature. The phases were separated and the aqueous phase was extracted with ethyl acetate (100 ml). The combined organic phases was dried (MgSO4) and the solvent evaporated in vacuo to give 25.9 g (99%) of 3-methoxypropiophenone.

WORKUP

后处理

  1. additionWhen addition
  2. stirringthe mixture was stirred for 1 h at room temperature
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with ethyl acetate (100 ml)
  5. dry with materialThe combined organic phases was dried (MgSO4)
  6. customthe solvent evaporated in vacuo