反应详情

温度

-78 °C

To a solution of 1-(3-fluoropyridin-2-yl)-3-oxocyclobutanecarbonitrile (231 g, 1.22 mol) in a mixture of DCM (2 L) and MeOH (200 mL) was added NaBH4 portionwise at −78° C. The reaction mixture was stirred at −78° C. for 1 h and quenched with a mixture of methanol and water (1/1). The organic layer was washed with water (500 mL×3), dried over Na2SO4, and concentrated. The residue was purified on silica gel (50% EtOAc/hexanes) to provide the title compound as an amber oil (185.8 g, 77.5%). LRMS (M+H+) m/z 193.2.

1. customquenched with a mixture of methanol and water (1/1)
2. washThe organic layer was washed with water (500 mL×3)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe residue was purified on silica gel (50% EtOAc/hexanes)