反应详情

温度

-78 °C

0.93 g (5 mmol) of 2-amino-4'-methylacetophenone hydrochloride was suspended in 30 ml of toluene in a 50-ml stainless steel autoclave. To the suspension was then added 0.79 g (10 mmol) of pyridine. The suspension was then cooled to a temperature of -78° C. To the suspension was then added about 0.5 g (9.6 mmol) of cyanogen which had been cooled and solidified at a temperature of -78° C. The autoclave was then sealed. The suspension was heated at a temperature of 100° C. for 2.5 hours, and then allowed to cool. The content was then taken out of the autoclave. The reaction mixture was then extracted with ethyl acetate and water. The resulting organic phase was dried over anhydrous sodium sulfate, and then subjected to silica gel column chromatography to obtain 0.48 g (yield: 52 %) of 2-cyano-4-(p-tolyl)imidazole.

1. temperaturehad been cooled
2. customsolidified at a temperature of -78° C
3. customThe autoclave was then sealed
4. temperatureThe suspension was heated at a temperature of 100° C. for 2.5 hours
5. temperatureto cool
6. extractionThe reaction mixture was then extracted with ethyl acetate and water
7. dry with materialThe resulting organic phase was dried over anhydrous sodium sulfate