p-Toluenesulfonic acid → 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

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence