反应详情

4-Bromobenzoic acid (9.98 kg, 48 mol) was suspended in 40 kg of methanol. Sulfuric acid (2 kg, 20 mol) was added and the mixture was heated under reflux for approximately 5 hours. The mixture was cooled over 10 hours to -10° C. and allowed to stand for 5 hours giving a crystalline product. The product was isolated by filtration and the filter cake was washed with methanol (2×3 L). Drying gave methyl 4-bromobenzoate (9.97 kg, 42 mol), m.p. 78°-78.7° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for approximately 5 hours
3. temperatureThe mixture was cooled over 10 hours to -10° C.
4. customgiving a crystalline product
5. customThe product was isolated by filtration
6. washthe filter cake was washed with methanol (2×3 L)
7. customDrying