反应详情

A solution of 1-(methylsulfonyl)-3,5-dinitro-benzene (1 g; 4 mmol) in methanol (80 ml) and toluene (20 ml) was treated with a solution of sodium hydrogensulfide-hydrate (227 mg; 4 mmol) in 20 ml methanol. The mixture was then refluxed for 3 hours additional 500 mg sodium hydrogensulfide-hydrate were added and refluxed for an additional hour. After cooling, the precipitate was filtrated and the filtrate concentrated. The residual was crystallized from methanol. 500 mg (2.31 mmol; 57% yield) of a yellow solid were obtained.

1. additionwere added
2. temperaturerefluxed for an additional hour
3. temperatureAfter cooling
4. filtrationthe precipitate was filtrated
5. concentrationthe filtrate concentrated
6. customThe residual was crystallized from methanol
7. custom500 mg (2.31 mmol; 57% yield) of a yellow solid were obtained