HRID342690

反应详情

EQUATION

反应方程式

HRID 342690 的结构方程式

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

  1. concentrationconcentrated in vacuo
  2. customto remove methanol
  3. additiondiluted with 10% aqueous sodium bicarbonate (100 mL)
  4. extractionextracted with ethyl acetate (2×150 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated