反应详情

To 1.39 g (6.37 mmol) of 2,7-dinitronaphthalene (124) was added 25 mL of concentrated HCl and 15 mL of ethanol. Then, 9.6 g (50.9 mmol) of tin (II) chloride was added and the reaction was heated at 78 C for 24 hours. The reaction was made basic with NaOH and extracted with ethyl acetate. The ethyl acetate layer was dried (MgSO4), filtered, and the volatiles removed by rotary evaporation. The product was purified by silica gel column chromatography eluting with 1% methanol in dichloromethane. This provided 0.965 g of compound 125.

1. temperaturethe reaction was heated at 78 C for 24 hours
2. extractionextracted with ethyl acetate
3. dry with materialThe ethyl acetate layer was dried (MgSO4)
4. filtrationfiltered
5. customthe volatiles removed by rotary evaporation
6. customThe product was purified by silica gel column chromatography
7. washeluting with 1% methanol in dichloromethane