反应详情

14 ml of a 3M solution of ethylmagnesium bromide in diethyl ether were added dropwise at 10° C. under an atmosphere of nitrogen to a solution of 8.33 g of 2-butyl-1-tritylimidazole-4,5-dicarbonitrile [prepared as described in Preparation 5(i)] in 83 ml of tetrahydrofuran, and the resulting mixture was stirred at room temperature for 3 hours. At the end of this time, a mixture of a saturated aqueous solution of ammonium chloride and ethyl acetate was added to the reaction mixture, whilst ice-cooling. The ethyl acetate layer was separated, washed with water and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure. The crystalline product thus obtained was washed with diisopropyl ether, to give 4.56 g of the title compound, melting at 140°-143° C. (softening at 83° C.).

1. additionwas added to the reaction mixture, whilst ice-
2. temperaturecooling
3. customThe ethyl acetate layer was separated
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was then removed by distillation under reduced pressure
7. customThe crystalline product thus obtained
8. washwas washed with diisopropyl ether