HRID1384835

反应详情

EQUATION

反应方程式

HRID 1384835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.5 g (66.1 mmol) of sodium borohydride are added to a solution of 4.04 g (10.6 mmol) of ethyl 7-chloro-5-methyl-4-oxo-3-phenyl-3,5-dihydro-4H-pyridazino[4,5-b]-indole-1-carboxylate in 150 ml of tetrahydrofuran. 2.25 ml of methanol are gradually added, with stirring, and then the mixture is heated at reflux for 5 hours. The mixture is poured onto an ice-cold 1 M hydrochloric acid solution and an insoluble product is separated by filtration on sintered glass, which product is washed with water and with diethyl ether and then dried. 3.3 g (9.7 mmol) of compound are isolated in the form of a white solid which is used as is in the following stage.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 5 hours
  3. customan insoluble product is separated by filtration on sintered glass, which product
  4. washis washed with water and with diethyl ether
  5. customdried