反应详情

温度

50 °C

A solution of 6-nitro-3-(N-propionyl-N-n-propylamino)chroman (17) (700 mg, 2.40 mmol) in glacial acetic acid (50 ml) was treated with zinc dust (1.0 g). The mixture was stirred at 50° C. for 90 minutes. The solution was filtered and acetic acid evaporated at reduced pressure. The product was dissolved in CH2Cl2 and washed with 5% -aqueous Na2CO3. The organic layer was separated, dried (Na2SO4) and the solvent was evaporated. The crude product was chromatographed on silica (60 g) , with CH2Cl2 --CH3OH (19:1) as eluant, yielding 350 mg (56%) of 6-amino-3-(N-propionyl-N-n-propylamino)chroman (18) as an oil.

1. filtrationThe solution was filtered
2. customacetic acid evaporated at reduced pressure
3. dissolutionThe product was dissolved in CH2Cl2
4. washwashed with 5% -aqueous Na2CO3
5. customThe organic layer was separated
6. dry with materialdried (Na2SO4)
7. customthe solvent was evaporated
8. customThe crude product was chromatographed on silica (60 g) , with CH2Cl2 --CH3OH (19:1) as eluant