Sodium hydride → 1-(3,5-Dibromo-4-nitropyrazol-1-yl)propan-2-ol

참여 물질

반응 조건

반응 단계

A mixture of 3,5-dibromo-4-nitropyrazole (2) (40.0 g; 147 mmol) in DMF (200 ml) was added over 15 minutes to a suspension of NaH (6.5 g, 162 mmol; 60% dispersion in oil, prewashed with hexane) in DMF (320 ml) with stirring and under an inert atmosphere. After stirring for 35 minutes, a solution of 1-bromo-2-propanol (26.8 ml; 221 mmol) in DMF (80 ml) was added dropwise. The reaction mixture was heated at 80° C. for 2 hours and the DMF was then evaporated off under reduced pressure. A mixture of DCM/water (480 ml, 2/1) was added. The organic phase was extracted with DCM (2×160 ml). The combined organic phases were washed with water (3×400 ml). The organic phase was dried over Na2SO4 and the solvent was evaporated off under reduced pressure. The 1-(3,5-dibromo-4-nitropyrazol-1-yl)-propan-2-ol was obtained as a white solid (23.3 g; 48%).

출처 및 근거