HRID1891015

反应详情

EQUATION

反应方程式

HRID 1891015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a stirred mixture of iron powder (0.5 g), ethanol (20 ml), water (1 ml) and concentrated hydrochloric acid (5 drops) at reflux was added N,N-Dimethyl-C-(3-nitro-phenyl)-methanesulfonamide (0.5 g). The mixture was then heated under reflux for a further 2 hours then basified with excess sodium carbonate solution, cooled to 60° C., then filtered. The filter cake washed with ethanol and the filtrate evaporated. The crude product was partitioned between ethyl acetate and water, separation and evaporation of the organic phase gave C-(3-Amino-phenyl)-N,N-dimethyl-methanesulfonamide, 0.4 g, sufficiently pure to use.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureThe mixture was then heated
  3. temperatureunder reflux for a further 2 hours
  4. filtrationfiltered
  5. washThe filter cake washed with ethanol
  6. customthe filtrate evaporated
  7. customThe crude product was partitioned between ethyl acetate and water, separation and evaporation of the organic phase