反应详情

温度

120 °C

A mixture of 6-chloro-pyridazine-3-carbonitrile (D4) (1.39 g, 9.95 mmol), 1-(3-fluoro-5-trifluoromethyl-benzyl)-piperidin-4-ylamine (D7) (2.5 g, 9.04 mmol) and diisopropylethylamine (2.63 ml, 14.92 mmol) in acetonitrile (2 ml) was stirred at 120° C. for 30 min, under microwave irradiation ((Biotage MW-oven). The mixture was then diluted with dichloromethane (50 ml) and extracted with a saturated solution of sodium carbonate. The organic layer was separated, dried (Na2SO4), filtered, evaporated in vacuo and the residue purified by column chromatography (silica gel; 0-2.5% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The residue precipitated from diisopropylether to yield E17 (2.76 g, 73%) as a solid. C18H17F4N5 requires 379. Found 380 (MH+); mp: 151.4° C.

1. extractionextracted with a saturated solution of sodium carbonate
2. customThe organic layer was separated
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo
6. customthe residue purified by column chromatography (silica gel; 0-2.5% ammonia in methanol (7M)/dichloromethane)
7. customThe desired fractions were collected
8. customevaporated in vacuo
9. customThe residue precipitated from diisopropylether