HRID342690
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a stirring solution of 4-[5-(2-methylthiopyrimidin-4-yl)-4-(3-trifluoromethylphenyl)-1H-imidazol-2-yl]piperidine-1-carboxylic acid benzyl ester (2.5 g, 0.0045 mole) in methanol (75 mL) at 20° C. was slowly added an aqueous solution (75 mL) of Oxone® (8.32 g, 0.0135 mole). The reaction was allowed to stir for 4 hours, concentrated in vacuo to remove methanol, diluted with 10% aqueous sodium bicarbonate (100 mL), and extracted with ethyl acetate (2×150 mL). The organic extracts were combined, dried over anhydrous sodium sulfate, filtered and concentrated to give the title compound (2.75 g).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customto remove methanol
- additiondiluted with 10% aqueous sodium bicarbonate (100 mL)
- extractionextracted with ethyl acetate (2×150 mL)
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated