反应详情

1-Bromo-4,5-dimethoxy-2-nitro-benzene (10 g) was suspended into ethanol (50 ml). To the reaction mixture was added the suspension of sodium sulfide (5 g) and sulfur (0.65 g) in ethanol (12 ml). The reaction mixture was refluxed 1.5 hour and then the resultant solid was filtered and washed with hot water and ethanol. The dry solid was slurried with acetic acid (60 ml) and acetanhydridi (35 ml). To the suspension was gradually added zinc (16.6 g) and the suspension was stirred at room temperature for 15 min before filtering off. The residue was evaporated to dryness. The product was purified by column chromatography using toluene-ethyl acetate-acetic acid 8:1:1 as the eluent.

1. additionTo the reaction mixture was added
2. temperatureThe reaction mixture was refluxed 1.5 hour
3. filtrationthe resultant solid was filtered
4. washwashed with hot water and ethanol
5. filtrationbefore filtering off
6. customThe residue was evaporated to dryness
7. customThe product was purified by column chromatography