反应详情

To a solution of 6-bromo-2-(N-(2-chloro-4-cyanobenzyl)acetamido)-3-nitropyridine (21.8 g) in ethanol (33 ml)-acetic acid (8.3 ml) was added iron powder (2.29 g) at room temperature, and the mixture was refluxed under heating for 2 hr. The reaction mixture was cooled, the insoluble matter was removed by filtration, and the solvent was evaporated. To the residue was added dichloromethane, and the product was extracted. The solvent was evaporated and the residue was purified by silica gel column chromatography (dichloromethane/methanol=30/1) to give the objective compound (1.90 g) as a pale-yellow powder.

1. temperaturethe mixture was refluxed
2. temperatureunder heating for 2 hr
3. temperatureThe reaction mixture was cooled
4. customthe insoluble matter was removed by filtration
5. customthe solvent was evaporated
6. additionTo the residue was added dichloromethane
7. extractionthe product was extracted
8. customThe solvent was evaporated
9. customthe residue was purified by silica gel column chromatography (dichloromethane/methanol=30/1)