反应详情

温度

120 °C

A mixture of 6-chloro-pyridazine-3-carbonitrile (D4) (1.32 g, 9.46 mmol), 1-(3,4,5-trifluoro-benzyl)-piperidin-4-ylamine (D8) (2.10 g, 8.6 mmol) and diisopropylethylamine (2.25 ml, 12.9 mmol) in acetonitrile (12 ml) was stirred at 120° C. for 20 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; 0-2% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The residue was precipitated from diisopropyl ether to yield E18 (2.210 g, 74%) as a solid. C17H16F3N5 requires 347. Found 348 (MH+); mp: 185° C.

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