反应详情

A mixture of N-(4-chloro-3-formyl-benzyl)-3,3,3-trifluoro-propionamide (840 mg, 3.00 mmol) and cyclopropylamine (0.320 mL, 4.51 mmol) in MeOH (30 mL) was heated to reflux for 4 h. The mixture was allowed to cool to rt. NaBH4 (170 mg, 4.51 mmol) was added in portions. The mixture was stirred for 1 h, and the solvents were removed under reduced pressure. The residue was diluted with EtOAc, and the resulting mixture was washed with aq. sat. NaHCO3 and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (CH2Cl2/MeOH 90:10) yielded the title compound (929 mg, 96%). LC-MS: tR=0.64 min; ES+: 321.05.

1. temperaturewas heated
2. temperatureto reflux for 4 h
3. customthe solvents were removed under reduced pressure
4. additionThe residue was diluted with EtOAc
5. washthe resulting mixture was washed with aq. sat. NaHCO3 and brine
6. dry with materiallayer was dried over MgSO4
7. filtrationfiltered
8. customthe solvents were removed under reduced pressure
9. customPurification of the crude by FC (CH2Cl2/MeOH 90:10)