HRID1902461

反应详情

EQUATION

反应方程式

HRID 1902461 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into 200 ml of benzene, 22.7 g (0.1 mol) of 3,4,5-trimethoxythiobenzamide and 16.0 g (0.12 mol) of 1-acetyl-1-chloroacetone were dissolved, and the solution was heated under a reflux condenser for 3 hours. The crystals, which separated out after cooling the reaction mixture, were recrystallized from methanol to obtain 24.5 g of pale yellow needle-like crystals of the product melting at 128° to 129° C. The yield was 79.8%. The method belongs to the above-mentioned method (a).

WORKUP

后处理

  1. temperaturethe solution was heated under a reflux condenser for 3 hours
  2. customThe crystals, which separated out
  3. temperatureafter cooling the reaction mixture
  4. customwere recrystallized from methanol