反应详情

A solution of sodium nitrite (7.3 g) in concentrated sulphuric acid was added to a stirred cooled solution of 4-bromo-2-fluoro-3-trifluoromethylaniline (27.4 g) in glacial acetic acid while maintaining the temperature below 15° C. The mixture was stirred at 10°-15° C. for one and a half hours then poured into a mixture of copper (I) chloride (10.5 g) in hydrochloric acid (5M). The mixture was stirred for one and a half hours then diluted with water, extracted with ether, washed with aqueous sodium hydroxide solution (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 6-bromo-3-chloro-2-fluorobenzotrifluoride (8.3 g) as a yellow oil b.p. 44°-45° C./2 mbar.

1. temperaturewhile maintaining the temperature below 15° C
2. stirringThe mixture was stirred for one and a half hours
3. extractionextracted with ether
4. washwashed with aqueous sodium hydroxide solution (2M), water
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customThe filtrate was evaporated to dryness
8. distillationthe residue was distilled