反应详情

A mixture of ethyl N-(3-nitropyridin-2-yl)glycinate (26 g) and 10% palladium on carbon (50% wet, 7.3 g) in AcOEt (250 mL) was hydrogenated under balloon pressure at room temperature for 8 h. The catalyst was removed by filtration. To the filtrate were added triethylamine (5.0 mL) and 10% palladium on carbon (50% wet, 7.3 g). The mixture was hydrogenated under balloon pressure at room temperature overnight. The mixture was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, eluted with 10%-50% AcOEt in hexane) to give the title compound (18 g).

1. customThe catalyst was removed by filtration
2. additionTo the filtrate were added triethylamine (5.0 mL) and 10% palladium on carbon (50% wet, 7.3 g)
3. waitThe mixture was hydrogenated under balloon pressure at room temperature overnight
4. concentrationThe mixture was concentrated under reduced pressure
5. customThe residue was purified by column chromatography (silica gel, eluted with 10%-50% AcOEt in hexane)