反应详情

A mixture of 3g of ethylthiooxamate, 4.25 g of 2-aminoacetophenone hydrochloride and 3.69 g of sodium acetate was dissolved in 20 mL of acetic acid and heated under reflux for 3 hr. The reaction mixture was allowed to cool to room temperature and the acetic acid removed by evaporation under reduced pressure. The residue was basified with aqueous sodium carbonate and extracted with 2×100 mL of ethyl acetate. The combined extracts were washed with 2×100 mL of brine, dried over anhydrous sodium sulfate and the solvent removed under reduced pressure to yield 2.8 g of ethyl 4-phenylimidazole-2-carboxylate as a solid which was used in the next step without further purification or characterization.

1. temperatureheated
2. temperatureunder reflux for 3 hr
3. customthe acetic acid removed by evaporation under reduced pressure
4. extractionextracted with 2×100 mL of ethyl acetate
5. washThe combined extracts were washed with 2×100 mL of brine
6. dry with materialdried over anhydrous sodium sulfate
7. customthe solvent removed under reduced pressure