反应详情

28.9 g (89 mmol) of 6-Chloro-1-cyclohexyl-7-nitro-2,3(1H,4H)-quinoxalinedione were dissolved in 300 ml of tetrahydrofuran/methanol/dimethylformamide (3:3:1) and, after addition of 3 g of palladium/carbon (10%), hydrogenated. The mixture was filtered, the carbon was washed with methanolic ammonia solution, and the combined filtrates were concentrated under reduced pressure. The residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1) to yield 2.2 g (8%) of product e1 and 18.5 g (80%) of product e2.

1. filtrationThe mixture was filtered
2. washthe carbon was washed with methanolic ammonia solution
3. concentrationthe combined filtrates were concentrated under reduced pressure
4. customThe residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1)