反应详情

To a solution of 4-[(2,2-dimethylpropyl)(2-oxoethyl)amino]-2-(trifluoromethyl)benzonitrile (0.882 g, 2.96 mmol) in MeOH (10 mL) at 0° C. was added NaBH4 (0.112 g, 2.96 mmol) in one portion and the mixture was stirred overnight, slowly warming to rt. The mixture was cooled to 0° C., sat'd NH4Cl (1 mL) was added and the mixture was concentrated in vacuo. The residue was partitioned between EtOAc/water and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (EtOAc/hexanes), affording 0.829 g of the title compound as a colorless syrup which solidified on standing: MS (ESI) m/z 301 (M+1).

1. temperatureThe mixture was cooled to 0° C.
2. concentrationthe mixture was concentrated in vacuo
3. customThe residue was partitioned between EtOAc/water
4. customthe layers were separated
5. washThe organic layer was washed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by flash chromatography (EtOAc/hexanes)