تفاعل #81305

معادلة التفاعل

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

المذيبات

diethyl ether

tetrahydrofuran

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.).

المصدر