反应详情

Phosgene (20% wt. in toluene; 0.49 mL, 0.92 mmol) was added to a solution of 3-amino-1-benzyl-3-[4-(benzyloxy)benzyl]azepan-2-one (76 mg, 0.18 mmol) and triethylamine (0.80 mL, 0.55 mmol) in dichloromethane (2 mL) at 0° C. After 30 min, the mixture was concentrated and redissoved in acetonitrile (5 mL). Diisopropylethylamine (0.060 mL, 0.37 mmol), and 4-(2-oxo-1,4-dihydroquinazolin-3(2H)-yl)piperidinium chloride (49 mg, 0.18 mmol) were added and the mixture was heated to reflux. After 1 h, the mixture was allowed to cool to ambient temperature and concentrated. Purification by silica gel chromatography (1% methanol/dichloromethane→5% methanol/dichloromethane gave the title compound (114 mg). MS 672 (M+1).

1. concentrationthe mixture was concentrated
2. temperaturethe mixture was heated to reflux
3. waitAfter 1 h
4. concentrationconcentrated
5. customPurification by silica gel chromatography (1% methanol/dichloromethane→5% methanol/dichloromethane