反应详情

2,6-Dichlorobenzoic acid (5.00 g, 26.2 mmol) was diluted in dimethylcarbonate (44 mL, 530 mmol). 1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU) (3.91 mL, 26.2 mmol) was added last. The reacted was refluxed for 2 days. Upon cooling, the solution was diluted with ethyl acetate and water. The aqueous layer was removed and the organic layer was washed with water, 2N HCl (2×'s), sat. NaHCO3 (2×'s), and twice with water. The organic layer was dried over sodium sulfate, filtered, and concentrated to yield 4.61 g (86%) of the desired compound as a clear oil.

1. temperatureThe reacted was refluxed for 2 days
2. temperatureUpon cooling
3. customThe aqueous layer was removed
4. washthe organic layer was washed with water, 2N HCl (2×'s), sat. NaHCO3 (2×'s), and twice with water
5. dry with materialThe organic layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated