HRID265640

反应详情

EQUATION

反应方程式

HRID 265640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

355,3 g (2 moles) of distilled 3-thiocyanato-5-chloro-2-pentanone are added into 360 cm3 of 85% phosphoric acid under stirring. The temperature of the reaction mixture is increased to 95° C. in water bath within about 1 hour and then it is stirred for half and hour between 95° to 100° C. The brown solution is cooled to 20° C. and poured into 660 cm3 of water. The precipitated beige crystals are removed by suction after a stirring for half an hour, washed neutral with water and dried in vacuo at a temperature of 60° C. 337 g (95%) of pale beige 2-hydroxy-4-methyl-5-(2-chloroethyl)thiazole are obtained, m.p.: 151°-152° C. After recrystallization from benzene the melting point is 157°-158° C.

WORKUP

后处理

  1. stirringit is stirred for half and hour between 95° to 100° C
  2. customThe precipitated beige crystals are removed by suction after a stirring for half an hour
  3. washwashed neutral with water
  4. customdried in vacuo at a temperature of 60° C