反应详情

A suspension of methyl 2,6-dichloro-4-(hydroxymethyl)benzoate (5.3 g, 22 mmol) in pyridine (20 mL) was treated with anhydrous lithium iodide (9 g, 67 mmol). The resulting reaction mixture was heated to reflux for 5 hours, cooled to room temperature and concentrated under vacuum. The residue was diluted with water and acidified with dilute hydrochloric acid (pH 2-3) and partitioned with ethyl acetate. The combined organic layer was washed with brine, dried over sodium sulfate, concentrated and the residue obtained upon triturating with diethyl ether afforded 2,6-dichloro-4-(hydroxymethyl)benzoic acid as a pale yellow solid (3.5 g, 70%).

1. customThe resulting reaction mixture
2. temperaturewas heated
3. temperatureto reflux for 5 hours
4. concentrationconcentrated under vacuum
5. additionThe residue was diluted with water
6. custompartitioned with ethyl acetate
7. washThe combined organic layer was washed with brine
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated
10. customthe residue obtained
11. customupon triturating with diethyl ether