HRID634958

反应详情

EQUATION

反应方程式

HRID 634958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 180.0 g (1.63 mols) of ammonium dithiocarbamate was added 1.5 liters of isopropyl alcohol, the mixture was stirred and then 268.9 g (1.63 mols) of ethyl 4-chloro-3-oxobutanoate was added dropwise to the mixture. After stirring the resultant mixture for 3 hours under refluxing, 300 ml of water was added to the reaction mixture, the mixture was cooled to room temperature and crystals formed were collected by filtration under a reduced pressure to obtain crude crystals. The crude crystals were recrystallized from ethyl acetate to obtain 188 g (yield 57%) of 4-ethoxycarbonylmethyl-2-mercaptothiazole.

WORKUP

后处理

  1. temperatureunder refluxing
  2. customcrystals formed
  3. filtrationwere collected by filtration under a reduced pressure
  4. customto obtain crude crystals
  5. customThe crude crystals were recrystallized from ethyl acetate