HRID444532

反应详情

EQUATION

反应方程式

HRID 444532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A hydrolysis mixture was prepared from 5.1 g. of dl-2-acetyl-5-acetamido-4,5,6,7-tetrahydro-2H-benzo[c]pyrrole, 50 g. of sodium hydroxide, 50 ml. of water, and 200 ml. of ethanol. The mixture was heated to refluxing temperature under a nitrogen atmosphere for about 16 hours and was then cooled. The cooled mixture was diluted with water. The alkaline aqueous mixture was extracted several times with methylene dichloride, the methylene dichloride extracts were combined and the combined extracts washed with saturated aqueous sodium chloride and dried. Evaporation of the solvent therefrom yielded a residue comprising dl-5-amino-4,5,6,7-tetrahydro-2H-benzo[c]pyrrol formed in the above reaction. A chloroform solution of the residue was filtered through 105 g. of alumina (grade II). Concentration of the resulting filtrate yielded 2.52 g. of a yellow solid comprising dl-5-amino-4,5,6,7-tetrahydro-2H-benzo[c]pyrrole.

WORKUP

后处理

  1. customA hydrolysis mixture was prepared from 5.1 g
  2. temperatureThe mixture was heated
  3. temperatureto refluxing temperature under a nitrogen atmosphere for about 16 hours
  4. temperaturewas then cooled
  5. extractionThe alkaline aqueous mixture was extracted several times with methylene dichloride
  6. washthe combined extracts washed with saturated aqueous sodium chloride
  7. customdried
  8. customEvaporation of the solvent