HRID1087227
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 5 hours
- concentrationThe mixture was concentrated to dryness
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water
- customdried
- customevaporated
- customThe residue (2.6 g) was purified by column chromatography on silica gel (70 g)
- washeluting with a mixture of chloroform and methanol (9:1)