反应详情

温度

0 °C

Ethyl 1-methylimidazole-2-carboxylate was carefully dissolved in 1000 mL of concentrated sulfuric acid cooled to 0° C. 90% nitric acid (1 L) was slowly added maintaining a temperature of 0° C. The reaction was then refluxed with an efficient condenser (−20° C.) in a well ventilated hood for 50 min. The reaction was cooled with an ice bath, and quenched by pouring onto 10 L ice. The resulting blue solution was then extracted with 20 L DCM, the combined extracts dried (sodium sulfate) and concentrated in vacuo to yield a tan solid which was recrystallized from 22 L of 21:1 carbon tetrachloride/ethanol. The resulting white crystals are collected by vacuum filtration.

1. temperaturemaintaining a temperature of 0° C
2. temperatureThe reaction was then refluxed with an efficient condenser (−20° C.) in a well ventilated hood for 50 min
3. temperatureThe reaction was cooled with an ice bath
4. customquenched
5. additionby pouring onto 10 L ice
6. extractionThe resulting blue solution was then extracted with 20 L DCM
7. dry with materialthe combined extracts dried (sodium sulfate)
8. concentrationconcentrated in vacuo
9. customto yield a tan solid which
10. customwas recrystallized from 22 L of 21:1 carbon tetrachloride/ethanol
11. filtrationThe resulting white crystals are collected by vacuum filtration