反应详情

To a solution of 2-chloro-3-nitropyridine (25.3 g) in EtOH (300 mL) were added ethyl 2-aminoacetate hydrochloride (28.7 g) and triethylamine (28.9 mL) at room temperature, and the mixture was refluxed for 1 day. The mixture was concentrated under reduced pressure. The residual crystals were removed by filtration and washed with AcOEt. The filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, eluted with 20%-70% AcOEt in hexane). The residual crystals were removed by filtration and washed with IPE. The filtrate was concentrated under reduced pressure to give the title compound (26.9 g).

1. temperaturethe mixture was refluxed for 1 day
2. concentrationThe mixture was concentrated under reduced pressure
3. customThe residual crystals were removed by filtration
4. washwashed with AcOEt
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe residue was purified by column chromatography (silica gel, eluted with 20%-70% AcOEt in hexane)
7. customThe residual crystals were removed by filtration
8. washwashed with IPE
9. concentrationThe filtrate was concentrated under reduced pressure