HRID359020

反应详情

EQUATION

反应方程式

HRID 359020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 75.0 g of 4-(trifluoromethyl)-phenylhydrazine in 500 ml of dry pyridine, cooled in an ice bath, was added dropwise, under nitrogen, 79.1 g of 2-fluorobenzoyl chloride. Upon completion of the addition, the ice bath was removed and the reaction mixture stirred at ambient temperature for 4 hours. The mixture was poured into water and a precipitate formed. Recrystallization of the precipitate from isopropyl alcohol-water, gave 108 g (84%) of 2-fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide as a solid. Subsequent recrystallization from isopropyl alcohol-water gave the analytical sample, mp 163°-165°.

WORKUP

后处理

  1. additionwas added dropwise, under nitrogen
  2. additionUpon completion of the addition
  3. customthe ice bath was removed
  4. additionThe mixture was poured into water
  5. customa precipitate formed
  6. customRecrystallization of the precipitate from isopropyl alcohol-water