反应详情

温度

50 °C

A clear solution of fumaric acid (0.223 g, 1.92 m mol) in methanol (3.0 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, (1.0 g, 1.92 m mol) in methanol (2.0 mL) at 22-25° C. and the resulting clear solution heated to 50° C. for 30 min. The mixture was cooled to 22-25° C. and ethylacetate (8.0 mL) charged drop wise into the reaction mass at 22-25° C. The solvent was stripped off and the reaction mass charged with fresh ethylacetate (8.0 mL). The reaction mass was then stirred for 60 min at 22-25° C. The resulting white color material was collected by filtration. The material was then 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 fumarate (0.91 g, 74.0%) as free flowing white color material.

1. customobtained
2. temperatureThe mixture was cooled to 22-25° C.
3. filtrationThe resulting white color material was collected by filtration
4. customThe material was then dried under reduced pressure with nitrogen gas
5. custombleed at 50° C.