反应详情

The residue 109A was dissolved in methanol (60 mL) and acetic acid (4 mL). Zinc metal (3.24 g, 49.6 mmol) was added and the mixture was stirred overnight at room temperature. The reaction was decanted off from unreacted zinc metal. The solvent was removed under vacuum and resuspended in ethyl acetate (30 mL). The precipitate was removed by filtration on a Buchner funnel with Celite. Solvent was removed from the filtrate and the residue was purified by column chromatography (2% MeOH/DCM) to give the product N1-(2-methoxyethyl)benzene-1,2-diamine (109B) as a red oil (422 mg, 72% yield over two steps). ESI-MS:m/z 167.4 (M+H)+.

1. customThe reaction was decanted off from unreacted zinc metal
2. customThe solvent was removed under vacuum
3. customThe precipitate was removed by filtration on a Buchner funnel with Celite
4. customSolvent was removed from the filtrate
5. customthe residue was purified by column chromatography (2% MeOH/DCM)