反应详情

温度

50 °C

0.50 g (0.00177 mol) of 4-nitro-2,6-dibromopyridine and 0.29 g (0.00177 mol) of benzenesulphinic acid sodium salt were dissolved in 17 ml of dimethylformamide and stirred at 50° C. for 1 hr. The solvent was removed and the residue was partitioned in water and ethyl acetate. The combined organic phases were washed with sat. sodium chloride solution and dried over MgSO4. After filtration and removal of the solvent the residue was chromatographed on silica gel with ethyl acetate/hexane 1:4 and subsequently dried in a high vacuum. There was obtained 0.59 g (88.5%) of 4-benzenesulphonyl-2,6-dibromopyridine as white crystals; m.p.: 134-135° C.

1. customThe solvent was removed
2. customthe residue was partitioned in water
3. washThe combined organic phases were washed with sat. sodium chloride solution
4. dry with materialdried over MgSO4
5. filtrationAfter filtration and removal of the solvent the residue
6. customwas chromatographed on silica gel with ethyl acetate/hexane 1:4
7. customsubsequently dried in a high vacuum