反应详情

温度

180 °C

A mixture of 6-chloro-4,5-dimethyl-pyridazine-3-carbonitrile (D11) (0.120 g, 0.72 mmol), 1-(3,5-difluoro-benzyl)-piperidin-4-ylamine (D5) (0.194 g, 0.86 mmol) and diisopropylethylamine (0.188 ml, 1.08 mmol) in acetonitrile was stirred at 180° C. for 20 min., under microwave irradiation (Biotage MW-oven), and then again at 180° C. for additional 30 min. Dichloromethane, water and a saturated solution of sodium carbonate were then added. The organic phase was separated, filtered over cotton and evaporated in vacuo. The residue was purified by column chromatography (silica gel; 0-1% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and the solvent evaporated in vacuo to yield E19 (0.108 g, 42%) as a solid. C19H21F2N5 requires 357. Found 358 (MH+).

1. waitagain at 180° C. for additional 30 min
2. customThe organic phase was separated
3. filtrationfiltered over cotton
4. customevaporated in vacuo
5. customThe residue was purified by column chromatography (silica gel; 0-1% ammonia in methanol (7M)/dichloromethane)
6. customThe desired fractions were collected
7. customthe solvent evaporated in vacuo