反应详情

A suspension of 3,5-dibromo nitrobenzene (J. Amer. Chem Soc., 1950, 72, 793) (1.0 g, 3.6 mmol) in methanol (30 ml) was added in portions to a stirred mixture of iron powder (0.52 g, 9.3 mmol) in a saturated solution of ammonium chloride (50 ml) at 60° C. The mixture was heated at reflux for 2 h, filtered and the filtrate extracted with dichloromethane (2×70 ml). The organic extract was dried (Na2SO4) and concentrated in vacuo to give the title compound (D7) as an oil (0.787 g, 87%), MH+ 250/252.

1. temperatureThe mixture was heated
2. temperatureat reflux for 2 h
3. filtrationfiltered
4. extractionthe filtrate extracted with dichloromethane (2×70 ml)
5. extractionThe organic extract
6. dry with materialwas dried (Na2SO4)
7. concentrationconcentrated in vacuo