反应详情

A solution of 6.4 g (14.3 mmol) of 9-bromo-1-(bromomethyl)-5-methyl-3-phenyl-3,5-dihydro-4H-pyridazino[4,5-b]indol-4-one, of 3.6 g (73 mmol) of sodium cyanide and of 0.57 g (1 mmol) of tetrabutylammonium bromide in a mixture of 170 ml of dichloromethane and of 85 ml of water is heated at reflux for 3 h with mechanical stirring. Separation is carried out by settling and the reaction mixture is extracted with dichloromethane. The organic phase is washed with water and dried over sodium sulphate and the solvent is evaporated under reduced pressure. 5.6 g (14.2 mmol) of product are obtained, which product is used as is in the following stage.

1. temperatureat reflux for 3 h with mechanical stirring
2. customSeparation
3. extractionthe reaction mixture is extracted with dichloromethane
4. washThe organic phase is washed with water
5. dry with materialdried over sodium sulphate
6. customthe solvent is evaporated under reduced pressure