Lithium hydroxide, monohydrate → 4-[1-[3-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid

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Reaction Conditions

Reaction Steps

Lithium hydroxide monohydrate (9.06 g, 215.94 mmol) was added to methyl 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoate (79.58 g, 196.31 mmol) in a mixture of MeOH (800 mL) and water (400 mL). The resulting suspension was stirred at 65° C. for 16 hours. The mixture was cooled to room temperature, the methanol evaporated and the aqueous residues diluted with water (600 mL), filtered then treated with 1M citric acid until precipitation ceased. The precipitate was collected by filtration, washed with water and dried to afford 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid (77 g, 101%) as a solid.

Provenance & Evidence