反应详情

In a round bottom flask equipped with a stirrer, a condenser and a nitrogen bubbler, 4-Chloro-2-hydroxymethyl-3,5-Lutidine (1 eq.) was dissolved in Dimethylformamide (3-9 volumes) and Methanol (1.5-4.5 volumes). Sodium methoxide (4 eq.) was added and the temperature was raised to (95-100ℑ C.). At the end of the reaction the solvent was distilled under vacuum. Water (2 volumes) was added to the residue and the product was extracted with dichloromethane (2×4 volumes). The combined organic extracts were dried over sodium sulfate, filtered and evaporated. The crude product, 2-hydroxymethyl-4-Methoxy-3,5-lutidine, was obtained in 55% yield.

1. customIn a round bottom flask equipped with a stirrer, a condenser
2. temperaturethe temperature was raised to (95-100ℑ C.)
3. customAt the end of the reaction the solvent
4. distillationwas distilled under vacuum
5. additionWater (2 volumes) was added to the residue
6. extractionthe product was extracted with dichloromethane (2×4 volumes)
7. dry with materialThe combined organic extracts were dried over sodium sulfate
8. filtrationfiltered
9. customevaporated