反应详情

Cyclopropylcarbonyl chloride (2.88 mL, 31.0 mmol) and Et3N (4.38 mL, 31.0 mmol) were added to a sol. of 3-(tert-butyl-dimethyl-silanyloxymethyl)-4-chloro-benzylamine (6.00 g, 20.9 mmol) in CH2Cl2 (125 mL). The mixture was stirred for 30 min at rt, and more CH2Cl2 was added. The mixture was washed with aq. sat. NH4Cl (2×), with aq. 1M NaOH (2×) and with brine (1×). The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (MeOH/CH2Cl2 1:19) yielded the title compound (6.10 g, 82%). LC-MS: tR=1.09 min; ES+: 395.42.

1. washThe mixture was washed with aq. sat. NH4Cl (2×), with aq. 1M NaOH (2×) and with brine (1×)
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 (MeOH/CH2Cl2 1:19)