反应详情

温度

60 °C

Treat a solution of 2-chloro-4-iodo-5-methoxymethoxy-pyridine (8.1 g, 27 mmol) in THF (40 mL) with 3 N HCl (61 mL). Heat the resulting mixture to 60° C. for 3 h. Cool the mixture to RT and adjust the pH to 7 by the slow addition of saturated aqueous sodium bicarbonate solution. Extract the mixture with three portions of ethyl acetate. Combine the organic extracts and dry over sodium sulfate, filter, and concentrate in vacuo to give the title compound 6.8 g (98%) as a brown solid. 1H NMR (400 MHz, DMSO-d6) δ 11.04 (s, 1H), 7.81-7.87 (m, 2H).

1. temperatureCool the mixture to RT
2. extractionExtract the mixture with three portions of ethyl acetate
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate in vacuo