反应详情

A solution of methyl 2-[(2-hydroxybenzoyl)amino]-2-methylpropanoate, K2CO3 (20 mmol, 2.68 g) and 2-(chloromethyl)oxirane (22 mmol, 2.03 g) in acetonitrile (60 ml) was stirred at reflux temperature overnight. The reaction mixture was diluted with EtOAc and washed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml). The organic phase was dried over Na2SO4 and concentrated at reduced pressure. The residue was purified on C18-column (H2O:CH3CN, 0.1M NH4OAc buffer, gradient 10% to 95% CH3CN) to give the subtitle compound (244 mg, 5% yield, two steps).

1. temperatureat reflux temperature overnight
2. washwashed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml)
3. dry with materialThe organic phase was dried over Na2SO4
4. concentrationconcentrated at reduced pressure
5. customThe residue was purified on C18-column (H2O:CH3CN, 0.1M NH4OAc buffer, gradient 10% to 95% CH3CN)