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
- 150 °C
PROCEDURE
实验过程
A mixture of 2-(4-(4-cyano-1-methyl-1H-[1,2,3]triazolo[4,5-c]pyridin-6-yl)-2-(trifluoromethyl)phenoxy)ethyl methanesulfonate (0.15 g) and 1-(6-methylpyridin-2-yl)piperazine (0.361 g) in N-methylpyrollidine (2 ml) was heated at 150° C. under microwave condition for 30 minutes. Solvent removed under vacuum and residue dissolved in methanol (1 ml) and purified by basic prep HPLC to give methyl-6-(4-(2-(4-(6-methylpyridin-2-yl)piperazin-1-yl)ethoxy)-3-(trifluoromethyl)phenyl)-1H-[1,2,3]triazolo[4,5-c]pyridine-4-carbonitrile (0.0132 g). 1H NMR (MeOD) δ: 8.45 (m, 3H), 7.43 (m, 2H), 6.57 (m, 2H), 4.46 (s, 3H), 4.41 (m, 2H), 3.35 (m, 3.35), 2.97 (m, 2H), 2.78 (m, 4H), 2.35 (s, 3H). MS m/z 523.2 (M+H).
WORKUP
后处理
- customSolvent removed under vacuum and residue
- dissolutiondissolved in methanol (1 ml)
- custompurified by basic prep HPLC