反应详情

温度

140 °C

Iron (0.35 g) was added to 1chloro-4-nitrobenzene (15.8 g) at 140° C., bromine (2.8 ml) was added dropwise and the mixture heated to 140° C. for 1 hour. Two further additions of iron and bromine were made at 1 hour intervals followed by a final addition of iron (0.07 g) and heating to 140° C. for 1 hour. The reaction mixture was allowed to cool to room temperature, added to sodium metabisulfite solution (200 ml) and stirred for 30 min. The solution was extracted with dichioromethane (×4), washed with aqueous sodium metabisulfite and water then dried (MgSO4) to give an oil which was used in the next step without further purification.

1. temperatureheating to 140° C. for 1 hour
2. temperatureto cool to room temperature
3. extractionThe solution was extracted with dichioromethane (×4)
4. washwashed with aqueous sodium metabisulfite and water
5. dry with materialthen dried (MgSO4)
6. customto give an oil which
7. customwas used in the next step without further purification