反应详情

温度

60 °C

To 21 g of conc. nitric acid was dropwise added 28 g of conc. sulfuric acid at 0° C., and the mixture was heated at 60° C. At intervals of 3 minutes, 10 g of 1-chloro-2-difluoromethoxy-5-fluorobenzene was added in 5 portions to the mixture, which was kept at 60° C. for half an hour. After cooling, the reaction mixture was poured on ice water and shaken with chloroform. The chloroform layer was washed with water, dried and concentrated. The residue was chromatographed on a column of silica gel, eluting with n-hexane-ethyl acetate (100:15 v/v). The eluate was concentrated to give 11 g of the titled compound XII-1.

1. customat 0° C.
2. waitwas kept at 60° C. for half an hour
3. temperatureAfter cooling
4. additionthe reaction mixture was poured on ice water
5. washThe chloroform layer was washed with water
6. customdried
7. concentrationconcentrated
8. customThe residue was chromatographed on a column of silica gel
9. washeluting with n-hexane-ethyl acetate (100:15 v/v)
10. concentrationThe eluate was concentrated