反应详情

A mixture of 0.041 g (0.38 mmol) of 5-amino-1H-pyrazole-4-carbonitrile and 0.1 g (0.38 mmol) of N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-acetamide in 10 mL of glacial acetic acid was refluxed for 2.5 hours and then the solvent was removed by reduced pressure distillation. Dichloromethane (15 mL) and a saturated sodium bicarbonate solution (10 mL) were added to the resulting residue. The two layers were separated, and the aqueous layer was washed with 10 mL of dichloromethane. The organic layers were washed with 10 mL of water and dried over magnesium sulfate. The dichloromethane layer was evaporated to dryness to yield an oil which, in the presence of ethyl acetate, gave 95 mg of N-{2-fluoro-5-[3-cyano-pyrazolo[1,5-a]pyrimidin-7-yl]-phenyl}-N-methyl-acetamide as a solid (yield 81%).

1. temperaturewas refluxed for 2.5 hours
2. customthe solvent was removed by reduced pressure distillation
3. additionDichloromethane (15 mL) and a saturated sodium bicarbonate solution (10 mL) were added to the resulting residue
4. customThe two layers were separated
5. washthe aqueous layer was washed with 10 mL of dichloromethane
6. washThe organic layers were washed with 10 mL of water
7. dry with materialdried over magnesium sulfate
8. customThe dichloromethane layer was evaporated to dryness
9. customto yield an oil which