反应详情

To a suspension of 1.68 g (0.01 mol) of 1,4-dimethyl-5-carbethoxyimidazole in 10 ml of water was added 0.8 g (0.02 mol) of sodium hydroxide. The mixture was heated to reflux for 30 min. Thereafter, 3.54 g (0.03 mol) of formaldehyde sodium bisulfite was added and heated to reflux for 4 hours. The water in the reaction mixture was removed, and the residue was extracted with isopropyl alcohol and filtered. The isopropyl alcohol extract was concentrated, and the residual solid recrystallized from ethyl acetate and filtered to afford 0.46 g of 1,4-dimethyl-5-hydroxymethylimidazole as a white powdered solid, m.p. 125°-127° C.

1. temperatureThe mixture was heated
2. temperatureto reflux for 30 min
3. temperatureheated
4. temperatureto reflux for 4 hours
5. customThe water in the reaction mixture was removed
6. extractionthe residue was extracted with isopropyl alcohol
7. filtrationfiltered
8. extractionThe isopropyl alcohol extract
9. concentrationwas concentrated
10. customthe residual solid recrystallized from ethyl acetate
11. filtrationfiltered