反应详情

To a solution of methyl 2,6-dichloro-4-cyanobenzoate (160 g, 694 mmol) in pyridine (1.5 L) at room temperature was added LiI (186 g, 1.39 mol). The mixture was heated under reflux for 2 hours, cooled to room temperature and concentrated under reduced pressure. The residue was treated with 2 N HCl (1 L) and the resulting precipitate was collected by filtration. The solid was recrystallized from DMF and water to give 2,6-dichloro-4-cyanobenzoic acid (110 g, yield: 73%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 8.18 (s, 2H). LCMS (ESI) m/z: 216.0 [M+H+].

1. temperatureThe mixture was heated
2. temperatureunder reflux for 2 hours
3. concentrationconcentrated under reduced pressure
4. additionThe residue was treated with 2 N HCl (1 L)
5. filtrationthe resulting precipitate was collected by filtration
6. customThe solid was recrystallized from DMF and water