反应详情

Trifluoroacetic acid (5 mL) was added to a solution of tert-butyl (3R)-1-(cyclopropylmethyl)-2-oxoazepan-3-ylcarbamate (257 mg, 0.91 mmol) in dichloromethane (10 mL). After 1 h, the mixture was concentrated and azeotroped with dichloromethane (3×) to give the crude amine. Diisopropylethylamine (0.070 mL, 0.40 mmol) was added to a solution of the crude amine (39 mg, 0.13 mmol) and 4-(2-oxo-1,4-dihydroquinazolin-3(2H)-yl)piperidine-1-carbonyl chloride (39 mg, 0.13 mmol) in 1,2-dichloroethane (2 mL) and the mixture was heated to reflux. After 1 h, the reaction was allowed to cool to ambient temperature. Purification by silica gel chromatography (1% methanol/dichloromethane→5% methanol/dichloromethane) gave the title compound (32 mg). MS 440 (M+1).

1. concentrationthe mixture was concentrated
2. customazeotroped with dichloromethane (3×)
3. customto give the crude amine
4. temperaturethe mixture was heated to reflux
5. waitAfter 1 h
6. customPurification by silica gel chromatography (1% methanol/dichloromethane→5% methanol/dichloromethane)