HRID1087227

反应详情

EQUATION

反应方程式

HRID 1087227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4'-acetyl-2'-(2,4-difluorophenylthio)methanesulfonanilide (2.5 g), ammonium acetate (5.4 g) and sodium cyanoborohydride (0.96 g) in methanol (50 ml) was refluxed for 5 hours. The mixture was concentrated to dryness. The residue was dissolved in ethyl acetate, washed with water, dried, and evaporated. The residue (2.6 g) was purified by column chromatography on silica gel (70 g) eluting with a mixture of chloroform and methanol (9:1) to give a white powder of 4'-(1-aminoethyl)-2'-(2,4-difluorophenylthio)methanesulfonanilide (0.84 g).

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. concentrationThe mixture was concentrated to dryness
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water
  5. customdried
  6. customevaporated
  7. customThe residue (2.6 g) was purified by column chromatography on silica gel (70 g)
  8. washeluting with a mixture of chloroform and methanol (9:1)