反应详情

温度

150 °C

To a mixture of 2,6-dibromo-3-nitrotoluene (1.0 g, 3.4 mmol) in 14 ml of N-methylpyrrolidinone was added 0.323 g of freshly prepared copper (I) cyanide. The reaction was stirred and heated at a temperature of 150° C. under a nitrogen atmosphere for a period of three hours. After this period, the reaction mixture was cooled to room temperature, diluted with dichloromethane, and washed with 10% aqueous sodium thiosulfate solution. The organic layer was separated, dried, and concentrated under vacuum to remove the solvent. The residue was chromatographed on silica gel, eluting with 20% ethyl acetate/80% hexane, to afford 0.293 g of 3-bromo-2-methyl-6-nitrobenzonitrile as a yellow-white crystalline solid, mp 116°-118° C.

1. waitAfter this period
2. temperaturethe reaction mixture was cooled to room temperature
3. washwashed with 10% aqueous sodium thiosulfate solution
4. customThe organic layer was separated
5. customdried
6. concentrationconcentrated under vacuum
7. customto remove the solvent
8. customThe residue was chromatographed on silica gel
9. washeluting with 20% ethyl acetate/80% hexane