HRID1058394

反应详情

EQUATION

反应方程式

HRID 1058394 的结构方程式

PROCEDURE

实验过程

A mixture of 2-chloro-4-[3-(3-hydroxyphenyl)-1-oxopropan-1-yl]benzoic acid, methyl ester (Example 94; 2.1 g, 6.6 mmol) and 1N sodium hydroxide solution was stirred for 4 h at room temperature. The solution was filtered through Celite and the filter cake was washed with water (5 mL). 1N hydrochloric acid solution (22 mL) was added to the stirred filtrate and the resulting mixture was stirred for 2 h and then filtered. The solid was washed with water, dried and crystallized from ether/hexane to afford 2-chloro-4-[3-(3-hydroxyphenyl)-1-oxopropan-1-yl]benzoic acid (1.59 g, 79% yield) as an off-white solid.

WORKUP

后处理

  1. filtrationThe solution was filtered through Celite
  2. washthe filter cake was washed with water (5 mL)
  3. addition1N hydrochloric acid solution (22 mL) was added to the stirred filtrate
  4. stirringthe resulting mixture was stirred for 2 h
  5. filtrationfiltered
  6. washThe solid was washed with water
  7. customdried
  8. customcrystallized from ether/hexane