反应详情

To a mixture of anhydrous cupric chloride (3.1 g) and 2 -bromo-3,4-difluoro-6-nitroaniline (4.6 g) in anhydrous acetonitrile (30 ml) was added t-butylnitrite (2.8 g) dropwise at 51° to 56° C. during 5 minutes. After stirring for 8 minutes at the same temperature, the reaction mixture was poured into chilled 10% diluted hydrochloric acid (30 ml) and extracted with benzene. The organic layer was washed with diluted hydrochloric acid and with water successively, dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified by silica gel chromatography eluting with dichloromethane-n-hexane (1:5) to give the title compound (4.0 g).

1. additionthe reaction mixture was poured
2. extractionextracted with benzene
3. washThe organic layer was washed with diluted hydrochloric acid and with water successively
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe resulting residue was purified by silica gel chromatography
7. washeluting with dichloromethane-n-hexane (1:5)