HRID1798995

反应详情

EQUATION

反应方程式

HRID 1798995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a mixture of ethanol (179 ml) and 2′-chloro-4′-fluoro-biphenyl-2-carboxylic acid ethyl ester (41.8 g) was added 2N aqueous sodium hydroxide solution (179 ml), and the mixture was stirred in an oil bath at 80° C. for 2 hr. The reaction mixture was cooled to room temperature, activated carbon (2.5 g) was added and the mixture was stirred for 2.5 hr. The activated carbon was filtered off through celite and washed with 50v/v % ethanol-water (100 ml). The filtrate was acidified with 2N hydrochloric acid (196 ml). Then, to this mixture was added water (33 ml) and the mixture was stirred at room temperature for 2 hr. This suspension was filtered, and the obtained solid was air-dried for 2 hr, and dried under reduced pressure at 60° C. to give the title compound (28.6 g, 2 steps 93%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. additionactivated carbon (2.5 g) was added
  3. stirringthe mixture was stirred for 2.5 hr
  4. filtrationThe activated carbon was filtered off through celite
  5. washwashed with 50v/v % ethanol-water (100 ml)
  6. additionThen, to this mixture was added water (33 ml)
  7. stirringthe mixture was stirred at room temperature for 2 hr
  8. filtrationThis suspension was filtered
  9. customthe obtained solid was air-dried for 2 hr
  10. customdried under reduced pressure at 60° C.