反应详情

To a solution of 2,4-dimethoxy-nitrobenzene (0.50 g) in chloroform (3 mL) is added dropwise a solution of bromine (0.23 g) in chloroform (1 mL) and the mixture is allowed to stir at room temperature for approximately 15 hours. Additional bromine (0.15 g) in chloroform (1 mL) is added and the reaction is stirred for an additional 4 hours. The mixture is then poured onto 5% aqueous sodium bisulfite and then extracted with chloroform. Pooled organic extracts are then washed successively with 5% aqueous sodium bisulfite then saturated sodium chloride, and then dried over anhydrous sodium sulfate. Removal of the solvent under reduced pressure and recrystallization of the residue from toluene provides the desired product as a yellow solid.

1. stirringthe reaction is stirred for an additional 4 hours
2. extractionextracted with chloroform
3. washPooled organic extracts are then washed successively with 5% aqueous sodium bisulfite
4. dry with materialsaturated sodium chloride, and then dried over anhydrous sodium sulfate
5. customRemoval of the solvent
6. customunder reduced pressure and recrystallization of the residue from toluene