反应详情

温度

0 °C

The mixture of 240 ml acetonitrile, 20.7 g (150 mmol) of K2CO3, 18 g (75 mmol) of ethyl-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate and 20.4 g (81.6 mmol) of 4-bromobenzylbromide was heated under reflux temperature for 7 h. The suspension is cooled, filtered and concentrated under reduced pressure to approximately ⅓ of the starting volume and stirred at about 0° C. for 1 h. The precipitate is filtered and dried at 35° C. for 1 h and afterwards suspended in 218 ml of water. The mixture is stirred for 2 h, filtered and dried again. 21.56 g of the crude product were isolated. Crude product was recrystallized from acetonitrile (87%, 55% of the synthesis)

1. temperaturewas heated
2. temperatureunder reflux temperature for 7 h
3. temperatureThe suspension is cooled
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure to approximately ⅓ of the starting volume
6. filtrationThe precipitate is filtered
7. customdried at 35° C. for 1 h
8. stirringThe mixture is stirred for 2 h
9. filtrationfiltered
10. customdried again