反应详情

温度

100 °C

A suspension of 18.7 g (57.89 mmol) of (+/−)-9-bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4a-diaza-benzocyclohepten-4-one in 520 mL of ammonia (7N solution in MeOH) in sealed tubes was stirred at 100° C. for 4 hours. The cooled solution was evaporated to remove solvent. After an acido-basic work-up and extraction with dichloromethane, the mixture was washed with saturated solution of sodium chloride. The organic phase was dried over sodium sulfate and concentrated. The residue was organised in diethyl ether to afford 6.70 g (44%) of product as a yellow solid.

1. customThe cooled solution was evaporated
2. customto remove solvent
3. extractionAfter an acido-basic work-up and extraction with dichloromethane
4. washthe mixture was washed with saturated solution of sodium chloride
5. dry with materialThe organic phase was dried over sodium sulfate
6. concentrationconcentrated