反应详情

A mixture of 4,6-dichloro-nicotinic acid methyl ester (6.0 g, 29 mmol), NaOMe (2.0 g, 37 mmol) in THF (60 mL) is stirred overnight at room temperature. The solvent is removed in vacuo. Ice-cold dilute HCl solution is added to the solution. The mixture is neutralized with NaHCO3 and extracted with EtOAc. The extract is washed with water, dried, and concentrated. The residue is triturated with hexane until solid is formed. The solid is collected by filtration to give 6-chloro-4-methoxy-nicotinic acid methyl ester. 1H NMR (CDCl3) 8.72 (s, 1H), 6.91 (s, 1H), 3.97 (s, 3H), 3.90 (s, 3H).

1. customThe solvent is removed in vacuo
2. additionIce-cold dilute HCl solution is added to the solution
3. extractionextracted with EtOAc
4. washThe extract is washed with water
5. customdried
6. concentrationconcentrated
7. customThe residue is triturated with hexane until solid
8. customis formed
9. filtrationThe solid is collected by filtration