反应详情

温度

0 °C

A solution of difluoro-pyrimidin-2-yl-acetic acid ethyl ester (1.75 g, 8.65 mmol), as prepared in the previous step (and containing undissolved green precipitate), in anhydrous absolute EtOH (18 mL) was stirred at 0° C. for 5 min, and was then treated with solid NaBH4 (655 mg, 17.3 mmol) in one slow steady portion at 0° C. Bubbles immediately formed, and the solution turned light amber. Stirring continued at 0° C. for 2 h, and the reaction was then quenched with half-saturated NH4Cl (40 mL) and extracted with EtOAc (2×15 mL). The organic phases were combined, washed with saturated NaCl (1×10 mL), dried (Na2SO4), and concentrated to give the title compound as a yellow oil (696 mg, 50%).

1. customBubbles immediately formed
2. stirringStirring
3. waitcontinued at 0° C. for 2 h
4. customthe reaction was then quenched with half-saturated NH4Cl (40 mL)
5. extractionextracted with EtOAc (2×15 mL)
6. washwashed with saturated NaCl (1×10 mL)
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated