反应详情

温度

57.5 °C

A mixture of 9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (2.35 g, 0.01 mol; see WO 01/28992), methanesulfonic acid 2-{[3-(4-cyanophenyl)propyl]methanesulfonylamino}ethyl ester (3.7 g, 0.01 mol; see Preparation A above) and anhydrous K2CO3 (2.1 g, 0.015 mol) in dry acetonitrile (70 mL) was stirred under nitrogen atmosphere at 55-60° C. for 3 days. After filtration and concentration, the crude product was purified by column chromatography (silica gel: 60-120 mesh, eluent: petroleum ether-ethyl acetate, 50:50). Yield: 3.25 g (66%).

1. filtrationAfter filtration and concentration
2. customthe crude product was purified by column chromatography (silica gel: 60-120 mesh, eluent: petroleum ether-ethyl acetate, 50:50)