反应详情

A solution of 1-(6-chloropyridin-3-yl)-4,4-difluorocyclohexanecarbonitrile (2.02 mmol) in 20 mL THF was added to a solution of BH3 in THF (6.07 mmol, 1 M). After heating to reflux for 1 h, the reaction mixture was cooled in an ice bath before a 2N HCl solution was slowly added. The mixture was then heated to reflux for another 20 min. The reaction mixture was extracted twice with DCM, basified with 1N NaOH solution and extracted 3 times with DCM. The combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo to give the desired product as yellow oil.

1. temperatureAfter heating
2. temperatureto reflux for 1 h
3. additionwas slowly added
4. temperatureThe mixture was then heated
5. temperatureto reflux for another 20 min
6. extractionThe reaction mixture was extracted twice with DCM
7. extractionextracted 3 times with DCM
8. washThe combined organic layers were washed with brine
9. dry with materialdried over MgSO4
10. concentrationconcentrated in vacuo