HRID1734737

反应详情

EQUATION

反应方程式

HRID 1734737 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 two-necked flask was charged under nitrogen with 45 ml of dimethylformamide and 16 g of a 50% strength by weight aqueous sodium hydroxide solution. After addition of 15 g of 2-mercaptobenzoic acid, 18 g of chlorotrifluoroethane were passed in at 0° C. and the reaction mixture was then transferred into a stirred autoclave. The mixture was heated at 100° C. for 12 hours (maximum pressure: 2.5 bar), allowed to cool and the crude product was then precipitated by addition of concentrated hydrochloric acid. The dried crude product was recrystallized from hot formic acid, giving 5.3 g of 2-(2',2',2'-trifluoroethylthio)benzoic acid having a melting point of 226°-227° C.

WORKUP

后处理

  1. customwere passed in at 0° C.
  2. temperatureto cool
  3. customthe crude product was then precipitated by addition of concentrated hydrochloric acid
  4. customThe dried crude product
  5. customwas recrystallized from hot formic acid