HRID1076713

反应详情

EQUATION

反应方程式

HRID 1076713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thionylchloride (1.53 ml.) was added dropwise to a stirred cooled suspension of 2-(3-hydroxypropylamino)-3-phenyl-3H-indol-3-ol (3 g.) in chloroform (25 ml.). On completion of the addition the reaction was allowed to warm to room temperature and then heated under reflux for 45 minutes. The solvent and excess thionyl chloride were removed under reduced pressure and the resulting product crystallised from isopropanol-ether to give the title compound as its hydrochloride salt (2.72 g.). After two recrystallisations from isopropanol-ether the hydrochloride had a m.p. 210°-212°C. (Found C, 60.8; H. 5.6; N, 8.3. C17H17ClN20HCl requires C, 60.5; H, 5.4; N 8.3%).

WORKUP

后处理

  1. temperaturecooled
  2. additionOn completion of the addition the reaction
  3. temperatureheated
  4. temperatureunder reflux for 45 minutes
  5. customThe solvent and excess thionyl chloride were removed under reduced pressure
  6. customthe resulting product crystallised from isopropanol-ether