反应详情

A solution of 10.4 g of 2-butylimidazole-4,5-dicarbonitrile (prepared as described in Preparation 1) in 150 ml of methylene chloride was added dropwise in an atmosphere of nitrogen at 10°-15° C. to 100 ml of a 2M solution of t-butylmagnesium chloride in diethyl ether, and the mixture was stirred at the same temperature for 1 hour. 200 ml of ethyl acetate and 100 ml of aqueous potassium hydrogensulfate were then added dropwise to the reaction mixture, and the mixture was stirred at room temperature for 20 minutes. At end of this time, insoluble materials were removed by filtration, and the organic layer was separated, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was purified by column chromatography through silica gel, using a 1:3 by volume mixture of ethyl acetate and hexane as the eluent, to give 7.95 g of the title compound as crystals, melting at 135°-137° C.

1. stirringthe mixture was stirred at room temperature for 20 minutes
2. customAt end of this time, insoluble materials were removed by filtration
3. customthe organic layer was separated
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated by evaporation under reduced pressure
6. customThe residue was purified by column chromatography through silica gel
7. additionby volume mixture of ethyl acetate and hexane as the eluent