反应详情

温度

0 °C

To a solution of 2-bromo-4′-nitroacetophenone (30 g, 0.123 mol) in ethanol (200 mL) at 0° C. was added a solution of NaCN (18 g, 0.368 mol) in H2O (60 mL) dropwise over 1 h. Upon completion of the addition, the mixture was stirred at 0° C. for an additional hour and then diluted with H2O (200 mL). The solution was treated with 1N aq. HCl solution, to a pH of 2, and extracted with CH2Cl2 (2×500 ML). The combined organic layers were dried over Na2SO4 and concentrated by rotary evaporation. The residue was purified by flash chromatography on silica gel eluting with 1:1 hexane/EtOAc to obtain 2-cyano-4′nitroacetophenone as an orange solid.

1. additionUpon completion of the addition
2. extractionextracted with CH2Cl2 (2×500 ML)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated by rotary evaporation
5. customThe residue was purified by flash chromatography on silica gel eluting with 1:1 hexane/EtOAc