反应详情

To a solution of tert-butyl 4-[4-(methoxycarbonyl)-2-nitrophenyl]piperazine-1-carboxylate (200 mg, 0.547 mmol) in 1,4-dioxane-water (2:1) (6.0 mL), iron powder (76 mg, 1.37 mmol) and acetic acid (1 mL) were added under ice-cold conditions, and the mixture was stirred at room temperature overnight. The reaction solution was added water and a saturated aqueous solution of sodium hydrogen carbonate under ice-cold conditions, filtered through a pad of celite, and extracted with ethyl acetate. Then, the organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/acetone). The title compound (83 mg (yield 45%)) was obtained as a yellow oil.

1. filtrationa saturated aqueous solution of sodium hydrogen carbonate under ice-cold conditions, filtered through a pad of celite
2. extractionextracted with ethyl acetate
3. washThen, the organic layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe obtained residue was purified by silica-gel column chromatography (hexane/acetone)