反应详情

13.9 ml of borane-THF complex are provided under ice cooling. A solution of 2.0 g of 2-bromo-4-chlorobenzonitrile (Example 65A) in 60 ml of THF is added slowly. The reaction mixture is then heated for 1 h under reflux, cooled and under ice cooling 20 ml of 1N hydrochloric acid are added dropwise. The mixture is heated under reflux for 1 h and left to cool. For the work-up the solution is adjusted to an alkaline pH 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 is reacted further without purification.

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