反应详情

温度

20 °C

To a solution of 1-methyl-6-(6-(2-(piperidin-4-yl)ethoxy)-5-(trifluoromethyl)-pyridin-3-yl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile trifluoroacetate (200 mg) and N,N-diisopropylethylamine (310 μl) in acetonitrile (8 ml), 2-chloro-N,N-dimethylacetamide (77 μl, 91 mg) was added and the mixture stirred at 20° C. for 65 h. The reaction mixture was concentrated. The residue diluted with water (20 ml) and extrated with DCM (50 ml×3), combined DCM layer dried over sodium sulphate and solvent removed under reduced pressure. The residue was then purified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1 to 15:1), converted to hydrochloric acid salt using 2N hydrochloric acid in diethyl ether to give 1-methyl-6-(6-(2-(1-(2-dimethylamino-2-oxo-ethyl)piperidin-4-yl)ethoxy)-5-(trifluoromethyl)pyridin-3-yl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile hydrochloride (179 mg).

1. concentrationThe reaction mixture was concentrated
2. additionThe residue diluted with water (20 ml)
3. dry with materialdried over sodium sulphate and solvent
4. customremoved under reduced pressure
5. customThe residue was then purified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1 to 15:1)