反应详情

温度

120 °C

A mixture of 6-chloro-pyridazine-3-carbonitrile (D4) (1.74 g, 12.46 mmol), 1-(3,5-difluoro-benzyl)-piperidin-4-ylamine (D5) (2.35 g, 10.386 mmol) and diisopropylethylamine (2.71 ml, 15.58 mmol) in acetonitrile (30 ml) was stirred at 120° C. for 40 min., under microwave irradiation (Milestone MW-oven). Dichloromethane, water and a saturated solution of sodium carbonate were then added. The organic layers were filtered over cotton, evaporated in vacuo and the residue was purified by column chromatography (silica gel; 0-1.5% ammonia in methanol (7 M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The residue was precipitated in heptane to yield E15 (2.065 g, 60%) as a solid. C17H17F2N5 requires 329. Found 330 (MH+); mp: 187.9° C.

1. filtrationThe organic layers were filtered over cotton
2. customevaporated in vacuo
3. customthe residue was purified by column chromatography (silica gel; 0-1.5% ammonia in methanol (7 M)/dichloromethane)
4. customThe desired fractions were collected
5. customevaporated in vacuo
6. customThe residue was precipitated in heptane