反应详情

A mixture of tert-butyl 1,4-diazepane-1-carboxylate (24.52 mmol, 4.91 g), 2-(4-(bromomethyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (24.52 mmol, 8.26 g) and sodium hydrogencarbonate (36.8 mmol, 3.09 g) in acetonitrile (100 mL) was stirred for 24 hours then was concentrated under reduced pressure. Dichloromethane was added and the suspension was filtered. The filtrate was concentrated under reduced pressure. The residue was chromatographed on silica eluting with dichloromethane to dichloromethane/methanol (5%) to give the title compound (7.1 g). MS (ESI) m/z 457.2 [M+H]+

1. concentrationthen was concentrated under reduced pressure
2. additionDichloromethane was added
3. filtrationthe suspension was filtered
4. concentrationThe filtrate was concentrated under reduced pressure
5. customThe residue was chromatographed on silica eluting with dichloromethane to dichloromethane/methanol (5%)