反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a solution of tert-butyl 4-(2-(5-(4-cyano-1-methyl-1H-[1,2,3]triazolo[4,5-c]pyridin-6-yl)-3-(trifluoromethyl)pyridin-2-yloxy)ethyl)piperidine-1-carboxylate (1.15 g) in dichloromethane (10 ml) and acetonitrile (5 ml), trifluoroacetic acid (2 ml) was added and the mixture stirred at 20° C. for 1 h then solvent evaporated under reduced pressure. The resulting residue was dissolved in ethyl acetate (10 ml) and diethyl ether added dropwise until the mixture turned cloudy. The solution was allowed to stand for two hours. The desired product was collected by filtration and washed with ether, dried in vacuum oven to give 920 mg 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 (78%).
WORKUP
后处理
- customsolvent evaporated under reduced pressure
- dissolutionThe resulting residue was dissolved in ethyl acetate (10 ml)
- additiondiethyl ether added dropwise until the mixture
- waitto stand for two hours
- filtrationThe desired product was collected by filtration
- washwashed with ether
- customdried in vacuum oven