反应详情

3.70 g of sodium are dissolved in 375 ml of ethanol and then 14.6 g of imidazole-4,5-dinitrile and 16.5 ml of o-methylbenzyl chloride are added and the whole is heated under reflux for 8 hours. The whole is concentrated to dryness by evaporation under reduced pressure and the residue is taken up in dichloromethane, washed in succession with water and with saturated sodium chloride solution, dried over sodium sulphate and concentrated to dryness by evaporation. The crude product is purified by chromatography on silica gel with toluene/ethyl acetate (5:1) and crystallised from ethyl acetate/hexane. 1-(o-methylbenzyl)-imidazole-4,5-dinitrile having a melting point of 80°-81° is obtained.

1. temperaturethe whole is heated
2. temperatureunder reflux for 8 hours
3. concentrationThe whole is concentrated to dryness by evaporation under reduced pressure
4. washwashed in succession with water and with saturated sodium chloride solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated to dryness by evaporation
7. customThe crude product is purified by chromatography on silica gel with toluene/ethyl acetate (5:1)
8. customcrystallised from ethyl acetate/hexane