HRID462452

反应详情

EQUATION

反应方程式

HRID 462452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}-thioacetamide (0.44 g) and chloroacetone (0.30 g) in ethanol (30 ml) was heated under reflux for 7 hours and then evaporated. The residual oil was purified by chromatography on silica (t.l.c. grade, 10 g) using dichloromethane plus 0-10% v/v ethyl acetate as eluant. Appropriate fractions were combined and evaporated and the residue triturated with diisopropyl ether. The resulting solid was collected, washed with petroleum ether (b.p. 60°-80° C.) and dried to give the title compound (78 mg), m.p. 107°-110° C.

WORKUP

后处理

  1. temperatureunder reflux for 7 hours
  2. customevaporated
  3. customThe residual oil was purified by chromatography on silica (t.l.c. grade, 10 g)
  4. customevaporated
  5. customthe residue triturated with diisopropyl ether
  6. customThe resulting solid was collected
  7. washwashed with petroleum ether (b.p. 60°-80° C.)
  8. customdried