HRID46480

反应详情

EQUATION

反应方程式

HRID 46480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

30.0 g of N-(3,5-bis-trifluoromethyl-phenyl)-N'-methyl-thiourea were stirred in 100 ml of 1,2-dimethoxyethane and 10 ml of triethylamine, and then 22 g of a 30% strength aqueous glyoxal solution were added. The thiourea thereupon dissolved, the reaction being exothermic. The solution was stirred for a further 12 hours at 20° C. and was concentrated in vacuo and the residue was stirred with water and a little acetic acid. The reaction product, which had solidified, was filtered off, washed and dried. Yield 32.0 g; melting point: 133°-135° C. after recrystallisation from toluene.

WORKUP

后处理

  1. concentrationwas concentrated in vacuo
  2. stirringthe residue was stirred with water
  3. filtrationwas filtered off
  4. washwashed
  5. customdried
  6. custommelting point: 133°-135° C. after recrystallisation from toluene