HRID1927145
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
0.097 g of 1-nitro-5-(1-methyl-2,6-dioxopiperidin-3-yl)-5H-thieno(3,4-c)pyrrole-4,6-dione was dissolved in 10 mL of acetone; and a solution obtained by dissolving 0.239 g of Na2S2O4 in 10 mL of water was added. The reaction mixture was refluxed for 2 h, cooled, and 10 mL of water were added. The aqueous phase was extracted with ethyl acetate (3×30 mL), the organic phases were combined, washed with 40 mL of water and 40 mL of brine, dried over anhydrous MgSO4, filtered, and evaporated to dryness to remove the solvent. The remaining residue was purified on silica gel column chromatography to yield a solid (0.046 g). MS (m/z): 292 (M−1)+.
WORKUP
后处理
- customand a solution obtained
- additionwas added
- temperatureThe reaction mixture was refluxed for 2 h
- temperaturecooled
- extractionThe aqueous phase was extracted with ethyl acetate (3×30 mL)
- washwashed with 40 mL of water and 40 mL of brine
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- customevaporated to dryness
- customto remove the solvent
- customThe remaining residue was purified on silica gel column chromatography