HRID839679

反应详情

EQUATION

反应方程式

HRID 839679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A stirred mixture of 2-(4-methoxyphenyl)-2-methyl 5-hydroxy-6,7-dichloro-1-indanone (2.6 g., 0.0077 mole), potassium carbonate (2.14 g., 0.0154 mole) and ethyl bromoacetate (2.58 g., 0.0154 mole) in dimethylformamide (60 ml.) is warmed at 55°-60° C. for 2.5 hrs., then treated with water (60 ml.),-10N sodium hydroxide solution (3 ml., 0.03 mole) and heated at 100° C. for one hour. The reaction mixture is added slowly to crushed ice-water (600 ml.)-12N hydrochloric acid (20 ml.) to precipitate 1.69 g. of [1-oxo-2-(4-methoxyphenyl)-2-methyl-6,7-dichloro-5-indanyloxy]acetic acid which melts at 173°-175° C. after crystallization from nitromethane.

WORKUP

后处理

  1. temperatureis warmed at 55°-60° C. for 2.5 hrs
  2. additionThe reaction mixture is added slowly
  3. customto precipitate 1.69 g
  4. customof [1-oxo-2-(4-methoxyphenyl)-2-methyl-6,7-dichloro-5-indanyloxy]acetic acid which melts at 173°-175° C. after crystallization from nitromethane