反应详情

To a solution of EXAMPLE 1B (6.27 g, 26.8 mmol) and 3,3-diphenylacrylaldehyde (7.26 g, 34.8 mmol) in dichloromethane/methanol (30 mL/30 mL) was added acetic acid (0.6 mL) followed by addition of sodium triacetoxyborohydride (8.52 g, 40.2 mmol) at room temperature. The reaction mixture was stirred overnight at room temperature. The organic solvents were concentrated in vacuo and the residue was partitioned between dichloromethane and saturated aqueous sodium bicarbonate. The organic layer was washed with water and with brine, dried over magnesium sulfate, filtered and the solvent was evaporated in vacuo. The remaining residue was crystallized from acetonitrile.

1. concentrationThe organic solvents were concentrated in vacuo
2. customthe residue was partitioned between dichloromethane and saturated aqueous sodium bicarbonate
3. washThe organic layer was washed with water and with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customthe solvent was evaporated in vacuo
7. customThe remaining residue was crystallized from acetonitrile