反应详情

温度

145 °C

A mixture of ethyl 6-bromo-8-nitro-4-oxo-4H-1-benzopyran-2-carboxylate (5.0 g, 14.6 mmol), 10% palladium-on-charcoal (0.541 g), formic acid (7.90 ml) and N,N-dimethylformamide (42 ml) was stirred at 145° C. for 5.75 h under inert atmosphere. After this time the mixture was left to cool and the catalyst was removed by filtration, washing it with N,N-dimethylformamide. The resulting filtrate was evaporated to dryness and the obtained residue was purified by chromatography through a silica gel column. Eluting with hexane:chloroform, 85:15, 2.109 g of the title product were recovered (55% yield).

1. waitAfter this time the mixture was left
2. temperatureto cool
3. customthe catalyst was removed by filtration
4. washwashing it with N,N-dimethylformamide
5. customThe resulting filtrate was evaporated to dryness
6. customthe obtained residue was purified by chromatography through a silica gel column
7. washEluting with hexane
8. customchloroform, 85:15, 2.109 g of the title product were recovered (55% yield)