HRID2290326

反应详情

EQUATION

反应方程式

HRID 2290326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}-acetamide (6.8 g) and Lawesson's reagent (6.4 g) in acetonitrile (300 ml) was stirred at room temperature for 2.5 hours, filtered and evaporated. The residue was purified by chromatography on silica (80 g) using dichloromethane plus 0-10% v/v ethyl acetate as eluant. Appropriate fractions were combined and evaporated and the residual oil triturated with diethyl ether. The resulting solid was collected, washed with diethyl ether and dried to give the title compound (5.9 g), m.p. 149°-150° C.

WORKUP

后处理

  1. filtrationfiltered
  2. customevaporated
  3. customThe residue was purified by chromatography on silica (80 g)
  4. customevaporated
  5. customthe residual oil triturated with diethyl ether
  6. customThe resulting solid was collected
  7. washwashed with diethyl ether
  8. customdried