HRID1284031

反应详情

EQUATION

反应方程式

HRID 1284031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-ethoxy-1,3-dihydropyrrolo[4,3,2-de]isoquinoline (5 g, 25 mmoles), described in Example 5, ethanol (50 ml), 3-(dimethylamino)propylamine (2.7 g, 26.4 mmoles) and conc. HCl (12.5 ml, 29 mmoles) in 50 ml of ethanol is heated at reflux for 7 hours. Some ethanol is removed by distillation, then ether and saturated HCl in ethanol (2 ml) is added. The precipitate is collected. Recrystallization for ethanol-ethyl acetate (a small amount of HCl in ethanol being added) gives the hydrochloride salt of the title compound, mp 289° - 290°C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux for 7 hours
  3. customSome ethanol is removed by distillation
  4. additionether and saturated HCl in ethanol (2 ml) is added
  5. customThe precipitate is collected
  6. customRecrystallization for ethanol-ethyl acetate (a small amount of HCl in ethanol being
  7. additionadded)