反应详情

温度

90 °C

6-Chloro-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine (10.0 g, 44.93 mmol), 4-piperidone monohydrate hydrochloride (8.48 g, 49.43 mmol) and DIPEA (16.3 mL, 98.85 mmol) in DMF (100 mL) were stirred and heated at 90° C. for 1 hour. The DMF was then evaporated in vacuo and the residue purified by flash silica chromatography, eluting with 2% MeOH in DCM. Pure fractions were concentrated to give a pale yellow precipitate. The precipitate was collected by filtration, washed with ether and air dried to afford 1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-one (10.61 g, 83%) as a pale yellow solid.

1. customThe DMF was then evaporated in vacuo
2. customthe residue purified by flash silica chromatography
3. washeluting with 2% MeOH in DCM
4. concentrationPure fractions were concentrated
5. customto give a pale yellow precipitate
6. filtrationThe precipitate was collected by filtration
7. washwashed with ether and air
8. customdried