反应详情

温度

50 °C

To 1-chloro-4-iodo-2-nitrobenzene (1.27 g, 4.49 mmol) in methanol (20 ml) was added iron powder (1.25 g, 22 mmol) and the reaction heated to 50° C. A solution of ammonium chloride (1.92 g, 36 mmol) in water (10 ml) was added slowly and the reaction heated to 70° C. overnight. Reaction was cooled, filtered through celite, washed with methanol and solvent reduced in vacuo. The residue was purified by chromatography on silica gel (gradient of hexane to 10% ethyl acetate in hexane) to afford the title compound. MS (ES+) m/e 254 [M+H]+.

1. temperaturethe reaction heated to 70° C. overnight
2. customReaction
3. temperaturewas cooled
4. filtrationfiltered through celite
5. washwashed with methanol and solvent
6. customThe residue was purified by chromatography on silica gel (gradient of hexane to 10% ethyl acetate in hexane)