HRID541132

反应详情

EQUATION

反应方程式

HRID 541132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of ethyl 4′-chloro-2′-methyl-biphenyl-2-carboxylate (27.10 g), ethanol (60 ml) and 1N aqueous sodium hydroxide solution (120 ml) was stirred at 100° C. for 2 hr. To the reaction mixture was added 8N aqueous sodium hydroxide m solution (10 ml), and the mixture was further stirred at 100° C. for 1 hr. The reaction mixture was cooled to room temperature. The insoluble material was filtered off, and washed with 33 v/v % ethanol-water (100 ml). The filtrate was adjusted to pH 2 with formic acid (23 ml) and the mixture was stirred at room temperature for 1 hr. This suspension was filtered, and the obtained solid was air-dried for 1 hr and dried under reduced pressure at 60° C. to give the title compound (22.082 g, 91%).

WORKUP

后处理

  1. stirringthe mixture was further stirred at 100° C. for 1 hr
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationThe insoluble material was filtered off
  4. washwashed with 33 v/v % ethanol-water (100 ml)
  5. stirringthe mixture was stirred at room temperature for 1 hr
  6. filtrationThis suspension was filtered
  7. customthe obtained solid was air-dried for 1 hr
  8. customdried under reduced pressure at 60° C.