反应详情

A mixture of 4-bromo-3,5-dimethyl-benzonitrile (1.50 g), hydroxylamine hydrochloride (0.90 g), triethylamine (1.8 mL) and ethanol (30 mL) is stirred at reflux temperature for 4 h. After cooling to room temperature, the mixture is concentrated, the residue is taken up in water, and the resulting mixture is extracted with ethyl acetate. The combined extract is washed with brine, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 7:3→3:7) to give the title compound. LC (method 11): tR=0.73 min; Mass spectrum (ESI+): m/z=243/245 (Br) [M+H]+.

1. temperatureat reflux temperature for 4 h
2. concentrationthe mixture is concentrated
3. extractionthe resulting mixture is extracted with ethyl acetate
4. extractionThe combined extract
5. washis washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 7:3→3:7)