HRID1381889

反应详情

EQUATION

反应方程式

HRID 1381889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,2,2-Trichloroethylchloroformate (64 ml) was added dropwise to a stirred suspension of 5-methyl-2H-1,4-thiazin-3(4H)-one (50 g) in a mixture of acetonitrile (500 ml)-pyridine (75 ml) under ice-cooling. The mixture was stirred at room temperature for 1 hour and then, poured into cold water (1.5 l) The resulting precipitates were collected by filtration, recrystallized from ethanol to give 5-methyl-6-[1-(2,2,2-trichloroethoxycarbonyl)-1,4-dihydro-4-pyridinyl]-2H-1,4-thiazin-3(4H)-one (120 g, yield 80.7%) as pale yellow prisms.

WORKUP

后处理

  1. temperaturecooling
  2. customprecipitates
  3. filtrationwere collected by filtration
  4. customrecrystallized from ethanol