反应详情

A stirred solution of 1031 g (3.5 moles) of 2-bromo-4-fluoro-5-nitrophenyl methyl carbonate in 300 mL of 2.3N aqueous sodium hydroxide was heated to reflux and stirred for three hours. The hot reaction mixture was filtered through diatomaceous earth. Any material remaining in the reaction vessel was washed onto the filter cake with 1000 mL of water. The filtrate was cooled to 8°-10° C., and 560 mL of concentrated hydrochloric acid was added, with stirring, over one hour. The resultant solid was collected by filtration. Any material remaining in the reaction vessel was washed onto the filter cake with 1000 mL of water. The dried filter cake was recrystallized from toluene to give, in two crops, 543 g of 2-bromo-4-fluoro-5-nitrophenol, m.p. 124°-126° C.

1. temperatureto reflux
2. filtrationThe hot reaction mixture was filtered through diatomaceous earth
3. washwas washed onto the filter cake with 1000 mL of water
4. temperatureThe filtrate was cooled to 8°-10° C.
5. addition560 mL of concentrated hydrochloric acid was added
6. stirringwith stirring, over one hour
7. filtrationThe resultant solid was collected by filtration
8. washwas washed onto the filter cake with 1000 mL of water
9. filtrationThe dried filter cake
10. customwas recrystallized from toluene