反应详情

To a suspension of isonipecotamide (12.3 g, 96 mmol) in 200 mL of dichloromethane, was added, benzaldehyde (10.6 g, 100 mmol) and sodium triacetoxyborohydride (29.7 gm, 140 mmol) and the mixture was stirred at room temperature for 5 days. The thick white mixture was diluted with 100 mL water and extracted with EtOAc (2×20 mL) The aqueous phase was basified with 1N NaOH to pH 22 12. The resulting white precipitate was collected by suction filtration. The white solid was subsequently taken up in 50 mL of EtOAc, and was washed with 20 mL of brine, then dried (MgSO4), filtered and concentrated to give 10.84 g (50%) of the desired product.

1. additionwas added
2. extractionextracted with EtOAc (2×20 mL) The aqueous phase
3. filtrationThe resulting white precipitate was collected by suction filtration
4. washwas washed with 20 mL of brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated