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
- 55 °C
PROCEDURE
实验过程
To a solution of 3-(2-(4-(3-(2,6-dichloro-phenyl)-5-isopropyl-3-H-(1,2,3)triazol-4ylmethyoxy)-2-methyl-phenyl)-vinyl)-benzoic acid methyl ester (0.025 g, 0.046 mmol) in THF (3 mL) is added lithium hydroxide (0.005 g, 0.21 mmol). The reaction mixture is heated to 55° C. The reaction is determined to be incomplete due to the presence of starting material by TLC (1:1 hexane/ethyl acetate). An additional amount of lithium hydroxide (0.050 g) is added and the reaction is heated to 60° C. for 3 h. The reaction is quenched with aqueous 1 N HCl and is extracted with ethyl acetate. The organic layer is washed with brine, dried over sodium sulfate, filtered, and concentrated to give the title compound. ES/MS m/e 521.8 (M+1).
WORKUP
后处理
- temperaturethe reaction is heated to 60° C. for 3 h
- customThe reaction is quenched with aqueous 1 N HCl
- extractionis extracted with ethyl acetate
- washThe organic layer is washed with brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated