反应详情

温度

160 °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 (70 mg) and N,N-diisopropylethylamine (85 mg) in acetonitrile (2 ml), 1-chloro-2-methylpropan-2-ol (48 mg) and sodium iodide (19 mg) were added and heated in microwave at 160° C. for 0.5 h. The reaction mixture was concentrated then diluted with dichloromethane and water, extracted with dichloromethane and separated by hydrophobic frits, concentrated. Purified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1, 15:1, 12.5:1 to 10:1) then passed through Strata SCX column (1 g) to give 20.0 mg yellow amorphous as 6-(6-(2-(1-(2-hydroxy-2-methylpropyl)piperidin-4-yl)ethoxy)-5-(trifluoromethyl)pyridin-3-yl)-1-methyl-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile (31%).

1. concentrationThe reaction mixture was concentrated
2. additionthen diluted with dichloromethane and water
3. extractionextracted with dichloromethane
4. customseparated by hydrophobic frits
5. concentrationconcentrated
6. customPurified by Strata Si column (5 g, dichloromethane:methanol=1:0, 25:1, 15:1, 12.5:1 to 10:1)