HRID1041839

反应详情

EQUATION

反应方程式

HRID 1041839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

21.0 g (72.98 mmol) of 1-bromo-3-fluoro-4-(methylsulfanyl)-2-(trifluoromethyl)benzene were dissolved in 275 ml of absolute diethyl ether and cooled to −78° C. 54.8 ml (87.59 mmol) of a 1.6M solution of n-butyllithium in hexane were slowly added dropwise, and the resulting solution was stirred at −78° C. for 60 minutes. The reaction mixture was then added to freshly ground dry ice and slowly warmed to RT. Water was added, and the reaction mixture was made alkaline using 2M NaOH solution and washed with diethyl ether. The aqueous phase was then acidified with 51M HCl solution, causing the product to precipitate. The precipitate was filtered off with suction and dried under reduced pressure.

WORKUP

后处理

  1. temperatureslowly warmed to RT
  2. washwashed with diethyl ether
  3. customto precipitate
  4. filtrationThe precipitate was filtered off with suction
  5. customdried under reduced pressure