反应详情

To a solution of racemic 6-chloro-3-(3,3-dimethyl-1-nitromethyl-butyl)-1,3-dihydro-indol-2-one (3.8 g, 12 mmol) in methanol (80 mL) was added an aqueous solution (20 mL) of ammonium chloride (6.5 g, 122 mmol), followed by the addition of Zinc (Aldrich, activated) (8 g, 122 mmol). The reaction mixture was stirred at room temperature for 0.5 h. The mixture was filtered through a short pad of celite. The filtrate was concentrated to a small volume, then the residue was partitioned between ethyl acetate and water. The organic layer was separated, the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with saturated aqueous NaHCO3, brine, dried over MgSO4, and concentrated to give racemic 3-(1-aminomethyl-3,3-dimethyl-butyl)-6-chloro-1,3-dihydro-indol-2-one as a white foam (3.4 g, 99%)

1. filtrationThe mixture was filtered through a short pad of celite
2. concentrationThe filtrate was concentrated to a small volume
3. customthe residue was partitioned between ethyl acetate and water
4. customThe organic layer was separated
5. extractionthe aqueous layer was extracted with ethyl acetate
6. washwashed with saturated aqueous NaHCO3, brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated