反应详情

To a suspension of 4-bromo-3-chlorobenzoic acid (5.00 g, 21.2 mmol) in ethanol (50 mL) was added sulphuric acid (5 mL) and the resultant mixture heated to reflux for 60 h. The reaction was partitioned between ethyl acetate (50 mL) and water (50 mL). The aqueous layer was extracted with further ethyl acetate and the combined organic fractions dried (phase separator) and concentrated in vacuo to give the title compound as a brown oil/solid (5.09 g, 19.3 mmol). δH (d6-DMSO, 400 MHz): 8.06 (1H, d), 7.96 (1H, d), 7.80 (1H, dd), 4.33 (2H, q), 1.33 (3H, t). MS (ES): no mass ion observed.

1. temperatureto reflux for 60 h
2. customThe reaction was partitioned between ethyl acetate (50 mL) and water (50 mL)
3. extractionThe aqueous layer was extracted with further ethyl acetate
4. customthe combined organic fractions dried (phase separator)
5. concentrationconcentrated in vacuo