反应详情

13.9 ml (13.9 mmol) of borane-THF complex (1 M) are provided with ice cooling. Slowly a solution of 604 mg (2.8 mmol) 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. For the work up, the solution is rendered alkaline with 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 (450 mg, about 73% pure) is reacted further without purification.

1. custom13.9 ml (13.9 mmol) of borane-THF complex (1 M) are provided with ice cooling
2. temperatureThereafter the reaction mixture is heated
3. temperatureunder reflux for 1 h
4. temperaturecooled
5. extractionextracted with dichloromethane
6. dry with materialThe organic phase is dried over sodium sulfate
7. concentrationconcentrated on a rotary evaporator
8. customThe crude product (450 mg, about 73% pure) is reacted further without purification