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 CH2Cl2CH3OH (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 CH2Cl2CH3OH (19:1) as eluant