反应详情

温度

70 °C

Methyl 2,6-dichloroisonicotinate (2.62 g) was partially dissolved in ethanol (50 mL) and a freshly prepared solution of 0.72 mol/L solution of sodium ethanolate (17.7 mL) was added at room temperature and then heated at 70° C. for 3 hours. The reaction was neutralized by the addition of 2N hydrochloric acid (6.5 mL) and then concentrated. The resulting solid was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated. The crude reaction was purified by column chromatography using an eluant of 2-4% ethyl acetate/hexane to provide the title compound (1.7 g) with the following physical data.

1. concentrationconcentrated
2. customThe resulting solid was partitioned between ethyl acetate and water
3. washThe organic phase was washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude reaction
8. customwas purified by column chromatography