反应详情

2,3-difluoro-1,4-di(2-thienyl)-5,6-dinitro-benzene (3.0 g, 8.15 mmol), iron powder (5.5 g, 98 mmol) and acetic acid (100 ml) were stirred at 45° C. for 4 h. Then the mixture was poured into cold 5% NaOH solution (250 ml) and extracted with diethyl ether three times. The ether phase was washed with NaHCO3 solution, dried over MgSO4 and concentrated. Purification with column chromatograph afforded 2,3-difluoro-1,4-di(2-thienyl)-5,6-diamino-benzene as yellow powder (2.1 g, 84%). 1H and 19F NMR spectra were as expected.

1. extractionextracted with diethyl ether three times
2. washThe ether phase was washed with NaHCO3 solution
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customPurification with column chromatograph