反应详情

A mixture of 4-bromo-3-fluoro-phenylamine (2.85 g, 15 m mole), ferrous sulfate (0.95 g), glycerol (5.658 g, 4.5 ml), nitrobenzene (1.125 g, 0.93 ml) and concentrated sulfuric acid (2.61 mL) were heated gently. After the first vigorous reaction, the mixture was heated to reflux for 7 hours. Nitrobenzene was evaporated in vacuo. The aqueous solution was acidified with glacial acetic acid and dark brown precipitate separated, which was purified by flash chromatography (silica gel, petroleum/ethyl acetate=8/1) to return compound title as white crystals (1.44 g, 42.5%).

1. temperaturewere heated gently
2. customAfter the first vigorous reaction
3. temperaturethe mixture was heated
4. temperatureto reflux for 7 hours
5. customNitrobenzene was evaporated in vacuo
6. customseparated
7. customwhich was purified by flash chromatography (silica gel, petroleum/ethyl acetate=8/1)