HRID29117

反应详情

EQUATION

反应方程式

HRID 29117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
3.5 °C

PROCEDURE

实验过程

To a solution of ethyl 2-methyl-3-(4-methylphenyl)-2-propenoate (1002 g) in toluene (5371 ml) was added dropwise a 70% solution of dihydrobis(2-methoxyethoxy) sodium aluminate in toluene (2152 g) at 10° C. or below. The solution was stirred at 2 to 5° C. for 1 hr, a 10% solution of Rochel's salt (5968 ml) was added dropwise thereto at 20° C. or below and the solution was stirred at room temperature for 30 min. The toluene layer was fractionated, and washed with a 10% solution of Rochel's salt (2984 ml) and then washed with water. The solvent was distilled off to give the title compound as an oil (756 g, yield 93.9%).

WORKUP

后处理

  1. stirringat 20° C. or below and the solution was stirred at room temperature for 30 min
  2. washwashed with a 10% solution of Rochel's salt (2984 ml)
  3. washwashed with water
  4. distillationThe solvent was distilled off