反应详情

A mixture of methyl 6-amino-2-(methyloxy)-3-pyridinecarboxylate (2.1 g, 11.8 mmol) and iodine (15 g, 59 mmol) in N,N-dimethylformamide (50 ml) was stirred overnight at room temperature. The mixture was poured into water (200 ml) and extracted with ethyl acetate (50 ml×2). The combined organic layer was washed with saturated sodium bicarbonate, 20% aqueous thiosulphate and brine, dried over magnesium sulfate, and concentrated in vacuo gave a brown solid. The residue was suspended in diethyl ether and collected by filtration to afford 2.9 g (79%) of the title compound as a pale brown solid.

1. extractionextracted with ethyl acetate (50 ml×2)
2. washThe combined organic layer was washed with saturated sodium bicarbonate, 20% aqueous thiosulphate and brine
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customgave a brown solid
6. filtrationcollected by filtration