反应详情

温度

4 °C

A 50 ml 3-neck round bottom flask fitted with a condenser, thermometer and mechanical stirrer was charged with 3.0 g (14.66 mmol) of 4-ethoxy-3-nitropyridine hydrochloride, 6.1 g (79.9 mmol) of ammonium acetate and 6.7 ml of absolute ethanol. The reaction mixture was refluxed for approximately 24 hours and cooled to about 4° C. The pH of the solution was adjusted to 8.0 with base and the precipitated solid was collected by filtration. The product was rinsed with chilled ethanol and dried in vacuo at 50° C. to afford 2.41 g of 3-nitro-4-aminopyridine (and a small amount of ammonium acetate). The identity of the product was verified by NMR comparison to an authentic sample.

1. customA 50 ml 3-neck round bottom flask fitted with a condenser
2. temperatureThe reaction mixture was refluxed for approximately 24 hours
3. filtrationthe precipitated solid was collected by filtration
4. washThe product was rinsed with chilled ethanol
5. customdried in vacuo at 50° C.