反应详情

Trifluoroacetic anhydride (56.0 mL, 400 mmol) was added dropwise to a dichloromethane (500 mL) solution of 2-(4-bromophenoxymethyl)benzoic acid (112 g, 364 mmol) at room temperature. The mixture was stirred at room temperature for 2 hour, BF3.OEt2 (10 mL, 169.3 mmol) was then added thereto, and the mixture was stirred at room temperature for additional 2 hours. The reaction mixture was washed with a saturated aqueous sodium bicarbonate solution, and then with a saturated sodium chloride solution, the washed mixture was then dried over anhydrous sodium sulfate, and the solvents were distilled off under a reduce pressure. The residue was purified by column chromatography (hexane-ethyl acetate=3:2), to give 96.0 g (91%) of the captioned compound in the form of crystals.

1. stirringthe mixture was stirred at room temperature for additional 2 hours
2. washThe reaction mixture was washed with a saturated aqueous sodium bicarbonate solution
3. dry with materialwith a saturated sodium chloride solution, the washed mixture was then dried over anhydrous sodium sulfate
4. distillationthe solvents were distilled off under a reduce pressure
5. customThe residue was purified by column chromatography (hexane-ethyl acetate=3:2)