1-Chloro-4-nitrobenzene → 2-Bromo-1-chloro-4-nitrobenzene

Temperature

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

ORD record

ord-32e90c940a5a40799c9dd2f35051de30

Source dataset

uspto-grants-2000_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06022976