反应详情

温度

100 °C

15 g (81 mmol) of 2-amino-4'-methylacetophenone hydrochloride was measured out in a 200-ml four-necked flask. To the material was then added 121 ml (121 mmol) of a 1 mol/l N,N-dimethylformamide solution of cyanogen. The mixture was then stirred. To the mixture was then added 29.4 g (243 mmol) of N,N-dimethylaniline. The mixture was then heated at a temperature of 100° C. with stirring for 3 hours. N,N-dimethylaniline was then distilled off from the reaction mixture under a pressure of 30 mmHg. The reaction mixture was then allowed to cool to room temperature. 200 ml of water was then poured into the reaction mixture. The reaction mixture was acidified with hydrochloric acid, and a precipitate was recovered by filtration. The filtration residue was dissolved in 200 ml of a 5% aqueous solution of sodium hydroxide, and the solution was filtered. The filtrate was then acidified with hydrochloric acid. 2-Cyano-4-(p-tolyl)imidazole as a desired compound was then recovered by filtration. The material was then dried to obtain 12.43 g of a desired compound with a purity of 83.4% (yield: 70.0%).

1. stirringwith stirring for 3 hours
2. distillationN,N-dimethylaniline was then distilled off from the reaction mixture under a pressure of 30 mmHg
3. temperatureto cool to room temperature
4. addition200 ml of water was then poured into the reaction mixture
5. filtrationa precipitate was recovered by filtration
6. dissolutionThe filtration residue was dissolved in 200 ml of a 5% aqueous solution of sodium hydroxide
7. filtrationthe solution was filtered
8. filtration2-Cyano-4-(p-tolyl)imidazole as a desired compound was then recovered by filtration
9. customThe material was then dried