反应详情

3,6-Dimethoxy-benzene-1,2-diamine was synthesized by dissolving 6.0 g of 1,4-dimethoxy-2,3-dinitro-benzene (Eur. J. Org. Chem. 2006, 2786-2794) in 220 mL EtOH, evacuating 3 times with N2 and adding 600 mg of 10 wt % Pd/C. The reaction was stirred under a H2 atmosphere (balloon). Another 300 mg of 10 wt % Pd/C were added after 2 days and the mixture was stirred for another 24 h. Filtration over a pad of celite and washing with EtOH and EtOAc yielded after concentration in vacuo 4.3 g of 3,6-dimethoxy-benzene-1,2-diamine as black solid.

1. customevacuating 3 times with N2
2. additionadding 600 mg of 10 wt % Pd/C
3. additionAnother 300 mg of 10 wt % Pd/C were added after 2 days
4. stirringthe mixture was stirred for another 24 h
5. filtrationFiltration over a pad of celite
6. washwashing with EtOH and EtOAc
7. customyielded
8. concentrationafter concentration in vacuo 4.3 g of 3,6-dimethoxy-benzene-1,2-diamine as black solid