反应详情

To a solution of methyl (4-hydroxyphenyl)acetate (106 mg, 0.639 mmol) in 5 ml anhydrous dichloromethane at RT was added a solution of 2-{(1S,2R)-2-[1-(5-chloropyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanol (150 mg, 0.532 mmol) in 5 ml anhydrous dichloromethane, triphenylphosphine (polymer-bound, 419 mg, 1.21 mmol), and di-test-butyl azodicarboxylate (245 mg, 1.07 mmol). The reaction mixture was stirred at RT for 3 hours. It was filtered by Celite® and concentrated. The residue was purified by column chromatography on silica gel (50 g) using a gradient eluent of 0-50% ethyl acetate in hexanes (1000 ml) to afford the title compound. LC/MS (m/z) 430.3 (M+H)+.

1. filtrationIt was filtered by Celite®
2. concentrationconcentrated
3. customThe residue was purified by column chromatography on silica gel (50 g)