反应详情

温度

57.5 °C

A suspension of 1-(1-benzyl-piperidin-4-yl)-6-chloro-4-(8-oxa-3-aza-bicyclo[3.2.1]oct-3-yl)-1H-pyrazolo[3,4-d]pyrimidine (1.0 g, 2.3 mmol) and potassium carbonate (0.94 g, 6.8 mmol) in 1,2-dichloroethane (15 mL) was treated with methyl chloroformate (0.53 mL, 6.8 mmol) and then heated for two hours in a 55-60° C. oil bath. The mixture was filtered through a pad of diatomaceous earth, eluting with dichloromethane. The filtrate was concentrated to dryness under reduced pressure to furnish methyl 4-(4-(8-oxa-3-azabicyclo[3.2.1]octan-3-yl)-6-chloro-1H-pyrazolo[3,4-d]pyrimidin-1-yl)piperidine-1-carboxylate. MS (ES+): 407.5, 409.6 (M+H)+

1. filtrationThe mixture was filtered through a pad of diatomaceous earth
2. washeluting with dichloromethane
3. concentrationThe filtrate was concentrated to dryness under reduced pressure