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
- 40 °C
PROCEDURE
实验过程
A solution of 50 mg (0.13 mmol) of 4-(3-naphthalen-1-ylmethyl-2,3-dihydro-imidazo[1,2-a]pyridin-2-ylsulfanyl)-butyric acid methyl ester in 2 mL of THF is treated with a solution of 11 mg (0.26 mmol) of lithium hydroxide monohydrate in 1 mL of water at room temperature. The resulting mixture is heated to 40° C., and stirred at this temperature for 3 h. Then the reaction mixture is cooled to room temperature and concentrated in vacuo. The residue is diluted with water and neutralized with 1N HCl solution. The product is extracted with ethyl acetate, and the organic layer is separated. The organic layer is washed with water and brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is purified by flash chromatography eluting with 3˜10% methanol in dichloromethane solution to give the title compound. LCMS (ESMS): m/z 377 (M+H+)
WORKUP
后处理
- temperatureThen the reaction mixture is cooled to room temperature
- concentrationconcentrated in vacuo
- additionThe residue is diluted with water and neutralized with 1N HCl solution
- extractionThe product is extracted with ethyl acetate
- customthe organic layer is separated
- washThe organic layer is washed with water and brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue is purified by flash chromatography
- washeluting with 3˜10% methanol in dichloromethane solution