反应详情

温度

50 °C

is A clear solution of maleic acid (0.445 g, 3.84 m mol) in methanol (1.0 mL) was added to a clear solution of 6-(4-{4-[2-(4-acetylpiperazin-1-yl)ethoxy]phenyl}piperidin-1-yl)-3-(trifluoromethyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine, obtained as described in Example 5.5, (2.0 g, 3.84 m mol) in methanol (2.0 mL) at 22-25° C. and the resulting clear solution heated to 50° C. for 30 min. The reaction mass was cooled to 22-25° C. and ethylacetate (16.0 mL) added drop wise to the reaction mass at 22-25° C. The reaction mass was then stirred for 60 min at 22-25° C. The resulting white color material was collected by filtration and washed with ethylacetate (5.0 mL). The material was dried under reduced pressure with nitrogen gas bleed at 50° C. to afford the desired product 6-(4-{4-[2-(4-acetylpiperazin-1-yl)ethoxy]phenyl}piperidin-1-yl)-3-(trifluoromethyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine maleate (2.21 g, 90.0%) as free flowing white color material.

1. customobtained
2. temperatureThe reaction mass was cooled to 22-25° C.
3. filtrationThe resulting white color material was collected by filtration
4. washwashed with ethylacetate (5.0 mL)
5. customThe material was dried under reduced pressure with nitrogen gas
6. custombleed at 50° C.