反应详情

温度

120 °C

A mixture of 6-chloro-pyridazine-3-carbonitrile (D4) (0.130 g, 0.931 mmol), 1-(3-trifluoromethyl-benzyl)-piperidin-4-ylamine (D6) (0.241 g, 0.931 mmol) and diisopropylethylamine (0.243 ml, 1.4 mmol) in acetonitrile (3 ml) was stirred at 120° C. for 30 min., under microwave irradiation (Biotage MW-oven). Dichloromethane and water were added, and then the mixture washed with a saturated solution of sodium carbonate. The organic phase was filtered over cotton and the solvent was evaporated in vacuo. The residue was purified by column chromatography (silica gel; 0-2% ammonia in methanol (7M)/dichloromethane) to yield E16 (0.215 g, 64%) as a solid. C18H18F3N5 requires 361. Found 362 (MH+); mp: 170.3° C.

1. washthe mixture washed with a saturated solution of sodium carbonate
2. filtrationThe organic phase was filtered over cotton
3. customthe solvent was evaporated in vacuo
4. customThe residue was purified by column chromatography (silica gel; 0-2% ammonia in methanol (7M)/dichloromethane)