反应详情

温度

60 °C

To a solution of ethy 3-amino-6-bromo-pyridine-2-carboxylate (10 g, 40.8 mmol) in THF (50 ml) was added Ac2O (12 ml, 127.8 mmol) at ambient temperature then the solution was heated to 60° C. for 3 h. The solution was allowed to cool to ambient temperature then concentrated under reduced pressure and dissolved in ethyl acetate. This afforded the product in crystalline form. The mother liquor was purified using flash chromatography eluting with ethyl acetate/heptane, gradient, giving ethyl 3-acetamido-6-bromo-pyridine-2-carboxylate as a yellow solid.

1. temperatureto cool to ambient temperature
2. concentrationthen concentrated under reduced pressure
3. dissolutiondissolved in ethyl acetate
4. customThis afforded the product in crystalline form
5. customThe mother liquor was purified
6. washeluting with ethyl acetate/heptane, gradient