HRID1196896

反应详情

EQUATION

反应方程式

HRID 1196896 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.1 g. 6,7-diamino-4,4-dimethyl-1,2,3,4-tetrahydroquinolin-2-one and 2.8 ml. acetic anhydride were stirred in 50 ml. ethanol for 30 minutes at ambient temperature. 20 ml. concentrated hydrochloric acid were then added thereto and the reaction mixture refluxed for 18 hours. The solvent was removed in a vacuum and the residue was dissolved in water, rendered alkaline with ammonia, filtered off with suction and washed with water. After recrystallization from ethyl acetate, there were obtained 2.4 g. of the title compound; m.p. 290°-294° C.

WORKUP

后处理

  1. temperaturethe reaction mixture refluxed for 18 hours
  2. customThe solvent was removed in a vacuum
  3. dissolutionthe residue was dissolved in water
  4. filtrationfiltered off with suction
  5. washwashed with water
  6. customAfter recrystallization from ethyl acetate
  7. customthere were obtained 2.4 g