反应详情

A solution of 24.73 g (110.7 mmol) 6-methoxy-5-nitrobenzotrifluoride in 260 ml acetic acid and 130 ml of aqueous HBr solution (62%) was heated to reflux for 96 h, cooled down, evaporated and taken up in aqueous saturated NaHCO3 solution/Et2O (3×). The organic phases were washed with aqueous 10% NaCl, dried over sodium sulfate, and evaporated to dryness to yield 19.27 g of the title compound as yellow solid of mp. 103–104° C.

1. temperatureto reflux for 96 h
2. temperaturecooled down
3. customevaporated
4. washThe organic phases were washed with aqueous 10% NaCl
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness