反应详情

温度

23.5 °C

A clear solution of toluene-4-sulfonic acid (2.884 g, 15.0 m mol) in methanol (5.0 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, (3.9 g, 7.5 m mol) in methanol (8.0 mL) at 22-25° C. Ethylacetate (20.0 mL) was added drop wise to the resulting clear solution 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 methanol (105.0 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 di-tosylate (4.31 g, 67.0%) as free flowing white color material.

1. customobtained
2. filtrationThe resulting white color material was collected by filtration
3. washwashed with methanol (105.0 mL)
4. customThe material was dried under reduced pressure with nitrogen gas
5. custombleed at 50° C.