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温度

0 °C

To a solution of 3,5-difluoro-4-formylbenzonitrile (1.0 g, 6.0 mmol) in EtOH (15 mL) at 0° C. was added NaBH4 (113 mg, 0.5 equiv). After stirring 2 h at 0° C., the reaction mixture was quenched with water and concentrated under reduced pressure. The crude residue was dissolved in DCM, washed with brine, dried over Na2SO4 and concentrated to give 3,5-difluoro-4-(hydroxymethyl)benzonitrile as a solid. All material was used in the next step. 1H NMR (400 MHz, CDCl3) δ 7.29-7.15 (m, 2H), 4.82 (d, J=6.2, 2H), 2.02 (dd, J=12.0, 5.6, 1H); GC-MS (ES) m/z 169 (M).

1. customthe reaction mixture was quenched with water
2. concentrationconcentrated under reduced pressure
3. dissolutionThe crude residue was dissolved in DCM
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated