反应详情

温度

120 °C

A mixture of (1R*,2R*,5S*,6R*)-8-benzyl-2-{[3,5-bis(trifluoromethyl) phenyl]methoxy}-1-phenyl-8-azabicyclo[3.2.1]octan-6-carboxamide (Example 75; 250 mg, 0.44 mmol), chloroacetone (1 ml) and N,N-dimethylforamide (4 ml) was stirred at 120° C. for 24 hours. After cooling to room temperature the reaction mixture was diluted with diethyl ether (70 ml), washed with saturated aqueous NaHCO3, water and brine. The organic phase was dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (iso-hexane:ethyl acetate) to give the title compound (53 mg, 12%).

1. temperatureAfter cooling to room temperature the reaction mixture
2. washwashed with saturated aqueous NaHCO3, water and brine
3. dry with materialThe organic phase was dried (Na2SO4)
4. concentrationconcentrated
5. customThe residue was purified by chromatography on silica gel (iso-hexane:ethyl acetate)