HRID1674695

反应详情

EQUATION

反应方程式

HRID 1674695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

18.6 g iron powder in 198 mL ethanol and 1.93 mL conc. aq. hydrochloric acid were stirred for 30 minutes at room temperature. 7.8 g (27.3 mmol) (RS)-S-(3-nitrophenyl)-N-(isopropylcarbamoyl)-S-methylsulfoximide in 20 mL methanol were added. The mixture was stirred at 60° C. for 2 hours and filtered over a bed of silica gel. The residue was washed with hot ethanol. The combined filtrates were evaporated. The crude residue was purified by column chromatography (silica gel, dichloromethane:dichloromethane/ethanol 1:1) to give 4.53 g (65% yield) of the title compound.

WORKUP

后处理

  1. filtrationfiltered over a bed of silica gel
  2. washThe residue was washed with hot ethanol
  3. customThe combined filtrates were evaporated
  4. customThe crude residue was purified by column chromatography (silica gel, dichloromethane:dichloromethane/ethanol 1:1)