反应详情

温度

0 °C

The above partially purified bromide was dissolved in DMF (300 mL) and cooled to 0° C. Sodium acetate (18.0 g, 0.22 mol) was added. The mixture was stirred at 60° C. for 30 min. After cooling, the mixture was diluted with H2O and extracted with EtOAc. The EtOAc extract was washed with H2O (2×), dried over anhydrous MgSO4 and concentrated in vacuo. Chromatography over silica gel and elution with hexanes:EtOAc (9:1) yielded a front fraction containing 5-chloro-4-nitro-2-methylbenzonitrile and dibromide. Further elution with hexanes:EtOAc (2:1) gave the title compound (19.5 g, 47%) as a pale yellow solid.

1. temperatureAfter cooling
2. extractionextracted with EtOAc
3. extractionThe EtOAc extract
4. washwas washed with H2O (2×)
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated in vacuo
7. washChromatography over silica gel and elution with hexanes:EtOAc (9:1)
8. customyielded a front fraction
9. washFurther elution with hexanes:EtOAc (2:1)