反应详情

13.9 ml of borane-THF complex are provided with ice cooling. Slowly a solution of 2.0 g of 2-bromo-4-chlorobenzonitrile (Example 1A) in 60 ml of THF is added. Thereafter the reaction mixture is heated under reflux for 1 h, cooled, and 20 ml of 1N hydrochloric acid are added dropwise, with ice cooling. The mixture is heated under reflux for 1 h and allowed to cool. For the work-up, the solution is rendered alkaline using a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. The crude product is reacted further without purification.

1. custom13.9 ml of borane-THF complex are provided with ice cooling
2. temperatureThereafter the reaction mixture is heated
3. temperatureunder reflux for 1 h
4. temperaturecooled
5. temperatureThe mixture is heated
6. temperatureunder reflux for 1 h
7. temperatureto cool
8. extractionextracted with dichloromethane
9. dry with materialThe organic phase is dried over sodium sulfate
10. concentrationconcentrated on a rotary evaporator
11. customThe crude product is reacted further without purification