反应详情

A mixture of 4-(3,5-dimethyl-benzylsulfanyl)-nitrobenzene (0.35 g, 1.28 mmol) calcium chloride (0.071 g, 0.64 mmol) and iron powder (−325 mesh) (0.573 g, 10.3 mmol) in 4 ml water and 17 ml ethanol was heated at reflux under nitrogen for 4.5 h. The reaction mixture was then cooled to room temperature, filtered through Celite and the filtrate was concentrated under reduced pressure. The residual oil was purified by column chromatography, eluting with 9:1 hexane/ethyl acetate to yield the title compound as a yellowish oil (0.29 g, 91% yield). MS: 244.3 (M+1)

1. temperaturewas heated
2. temperatureat reflux under nitrogen for 4.5 h
3. filtrationfiltered through Celite
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residual oil was purified by column chromatography
6. washeluting with 9:1 hexane/ethyl acetate