反应详情

0.309 g of 1-nitryl-5-(2,6-dioxopiperidin-3-yl)-5H-thieno(3,4-c)pyrrole-4,6-dione was suspended in 20 mL of ethanol and 20 mL of water, and 0.7 g freshly-activated iron powder (washed with water after hydrochloric acid treatment) and 5 mL acetic acid were added and refluxed for 2 h. The reaction mixture was cooled and filtered. The filtered solution was evaporated to dryness; and the remaining residue was dissolved in 150 mL of ethyl acetate, washed with 40 mL of water and 40 mL of brine, dried over anhydrous MgSO4, filtered, and evaporated to dryness. The remaining residue was purified on silica gel column chromatography to obtain a solid (0.095 g).

1. temperaturerefluxed for 2 h
2. temperatureThe reaction mixture was cooled
3. filtrationfiltered
4. customThe filtered solution was evaporated to dryness
5. dissolutionand the remaining residue was dissolved in 150 mL of ethyl acetate
6. washwashed with 40 mL of water and 40 mL of brine
7. dry with materialdried over anhydrous MgSO4
8. filtrationfiltered
9. customevaporated to dryness
10. customThe remaining residue was purified on silica gel column chromatography