反应详情

Methyl chloroformate (1.98 mL, 25.2 mmol) was added to a sol. of 3-(tert-butyl-dimethyl-silanyloxymethyl)-4-chloro-benzylamine (6.00 g, 20.9 mmol) and DIPEA (7.33 mL, 42.0 mmol) in CH2Cl2 (100 mL) at rt. The mixture was stirred for 1 h at rt, and more CH2Cl2 was added. The mixture was washed with aq. sat. NH4Cl, aq. 1M NaOH, and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (EtOAc/heptane 1:5) yielded the title compound (5.39 g, 75%). LC-MS: tR=1.02 min; ES+: 344.38.

1. washThe mixture was washed with aq. sat. NH4Cl, aq. 1M NaOH, and brine
2. dry with materiallayer was dried over MgSO4
3. filtrationfiltered
4. customthe solvents were removed under reduced pressure
5. customPurification of the crude by FC (EtOAc/heptane 1:5)