反应详情

温度

100 °C

41.13 g (190.4 mmol) 1,7-dichloro-6-fluoro-isoquinoline (6) were dissolved in 670 ml of acetic acid. After addition of 148.8 g (1.90 mol) of ammonium acetate, the solution was stirred at 100° C. After 3 h, the solvent was removed under reduced pressure and the residue was poured into water. The aqueous phase was extracted three times with dichloromethane, the combined organic layer was washed with saturated sodium bicarbonate solution and brine, dried over sodium sulfate and evaporated to dryness. The crude product was crystallized from ethyl acetate/heptane to yield 14.85 g of the desired product. Another 4.5 g could be obtained upon evaporation and silica gel chromatography of the mother liquor.

1. customthe solvent was removed under reduced pressure
2. additionthe residue was poured into water
3. extractionThe aqueous phase was extracted three times with dichloromethane
4. washthe combined organic layer was washed with saturated sodium bicarbonate solution and brine
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness
7. customThe crude product was crystallized from ethyl acetate/heptane