反应详情

温度

50 °C

10% palladium on charcoal (3 g) was added to a suspension of 4-amino-6-benzyloxy-7-methoxy-2-[4-(4-morpholinecarbonyl)-1,4-diazepan-1-yl]quinazoline (16.35 g, 0.033 mol) in ethanol (800 ml) and the reaction stirred at 50° C. under a hydrogen atmosphere of 414 kPa (60 p.s.i.) for 72 hours. On cooling, the reaction mixture was filtered through Arbocel™, washed well with further ethanol and the filtrate concentrated under reduced pressure. The crude product was purified on silica gel eluting with a solvent gradient of 0.880 aqueous ammonia:methanol:dichloromethane (0.5:3.5:96 to 1:7:92, v/v) to give the subtitle compound as a white solid (7.1 g, 53%). Rf 0.17 (0.880 aqueous ammonia:methanol:dichloromethane 1:7:92, v/v). MS m/z 403 (MH)+.

1. temperatureOn cooling
2. filtrationthe reaction mixture was filtered through Arbocel™
3. washwashed well with further ethanol
4. concentrationthe filtrate concentrated under reduced pressure
5. customThe crude product was purified on silica gel eluting with a solvent gradient of 0.880 aqueous ammonia:methanol:dichloromethane (0.5:3.5:96 to 1:7:92