反应详情

To a solution of 0.290 g (0.73 mmol) of (+/−)-10-[(4-fluoro-2-methoxy-phenyl)-hydroxy-methyl]-2-pyrimidin-4-yl-7,8,9,10-tetrahydro-6H-pyrimido[1,2-α]azepin-4-one (example 4) in dichloromethane (14 mL) under argon at −78° C. was added 0.294 g of diethylaminosulfur trifluoride (1.83 mmol) diluted in 5 ml of dichloromethane. The reaction was allowed to increase to room temperature. The reaction was stirred at room temperature for 2 h; the mixture was quenched at 0° C. with the addition of methanol and stirred overnight. A saturated solution of ammonium chloride was added and the mixture was extracted with dichloromethane. The organic phase was washed with a saturated solution of sodium chloride and dried over sodium sulfate and concentrated. The residue was purified by flash chromatography (dichloromethane with 2% of methanol and 0.2% of ammonia) to afford 0.072 g (25%) of a white solid as an isomer mixture (95/5).

1. customthe mixture was quenched at 0° C. with the addition of methanol
2. stirringstirred overnight
3. additionA saturated solution of ammonium chloride was added
4. extractionthe mixture was extracted with dichloromethane
5. washThe organic phase was washed with a saturated solution of sodium chloride
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe residue was purified by flash chromatography (dichloromethane with 2% of methanol and 0.2% of ammonia)