Lithium hydroxide, monohydrate → 4-[1-[3-(Trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid
Reaktionsgleichung
O.[OH-].[Li+].[F:4][C:5]([F:32])([F:31])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:30]=[CH:29][C:24]([C:25]([O:27]C)=[O:26])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH:13]=[CH:14][C:9]2=[N:8][N:7]=1>CO.O>[F:32][C:5]([F:4])([F:31])[C:6]1[N:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][CH:18]([C:21]4[CH:30]=[CH:29][C:24]([C:25]([OH:27])=[O:26])=[CH:23][CH:22]=4)[CH2:17][CH2:16]3)[CH:13]=[CH:14][C:9]2=[N:8][N:7]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
Lithium hydroxide monohydrate (0.154 g, 3.66 mmol) was added to methyl 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoate (1.35 g, 3.33 mmol) in a mixture of methanol (30 mL) and water (15 mL). The resulting suspension was stirred at 50° C. for 16 hours. The mixture was cooled to room temperature, the methanol evaporated and the aqueous residue treated with 1M citric acid until precipitation ceased. The precipitate was collected by filtration, washed with water and dried to give 4-[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]benzoic acid (1.26 g, 97%) as a solid.
Aufarbeitung
- temperatureThe mixture was cooled to room temperature
- customthe methanol evaporated
- additionthe aqueous residue treated with 1M citric acid until precipitation
- filtrationThe precipitate was collected by filtration
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-176b20c597394fbe8dfe6d92c73707fb
- Quelldatensatz
- uspto-grants-2011_08
- Patentnummer
- US08003649B2
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