反应详情

温度

85 °C

Oxaldehyde (40% in water; 1.43 ml, 31.3 mmol) was added to a solution of 3-nitro-o-phenylene-diamine (600 mg, 3.9 mmol) in EtOH (15 ml) and the mixture was heated at 85° C. for 2 h. The solvent was removed in vacuo, the residue was diluted in water and the aqueous phase was extracted with DCM. The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent to give the title compound (666 mg, 97%).

1. customThe solvent was removed in vacuo
2. additionthe residue was diluted in water
3. extractionthe aqueous phase was extracted with DCM
4. dry with materialThe organic phase was dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent