HRID1493307

反应详情

EQUATION

反应方程式

HRID 1493307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of monoperphtalic acid in AcOEt (0.37 M solution; 20 ml) is added at 0° C. to a mixture of 2-(phenylthio) methyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine (3.5 g) and NaHCO3 (3 g) in AcOEt (20 ml). After 30 minutes the mixture is filtered and the eluate is washed with 1N solution of sodium thiosulfate (2×20 ml) and then with water (3×10 ml). The organic layer is dried on Na2SO4 and evaporated to dryness; the residue is purified by chromatography on SiO2 (hexane/AcOEt 85/15, as eluent) to give 3.5 g of 2-(phenylsulfinyl)methyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine, m.p. 160°-162° C.

WORKUP

后处理

  1. filtrationAfter 30 minutes the mixture is filtered
  2. washthe eluate is washed with 1N solution of sodium thiosulfate (2×20 ml)
  3. customThe organic layer is dried on Na2SO4
  4. customevaporated to dryness
  5. customthe residue is purified by chromatography on SiO2 (hexane/AcOEt 85/15, as eluent)