반응 #81305

반응 방정식

ethylmagnesium bromide

2-butyl-1-tritylimidazole-4,5-dicarbonitrile

2-butyl-1-tritylimidazole-4,5-dinitrile

ammonium chloride

ethyl acetate

→

title compound

2-Butyl-5-cyano-4-propionyl-1-tritylimidazole

용매

diethyl ether

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONwas added to the reaction mixture, whilst ice-
2. 2
   온도cooling
3. 3
   기타The ethyl acetate layer was separated
4. 4
   세척washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   기타The solvent was then removed by distillation under reduced pressure
7. 7
   기타The crystalline product thus obtained
8. 8
   세척was washed with diisopropyl ether

실험 절차

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.).

출처