反应 #2528265
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07728012B2
反应条件: temp:2.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 0.75 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC), 0.51 g of hydroxylbenzotriazole (HOBt) and 0.55 ml of triethylamine (Et3N) were successively added to a solution of 1.0 g of 2-(4-phenyl-1H-imidazol-1-yl)pyridine-3-carboxylic acid (3.77 mmol) in 50 ml of dichloromethane at 0-4° C., and the mixture was stirred at 0-4° C. for 1 hour. 0.9 g of 3-amino-2-hydroxy-4-phenylbutanamide hydrochloride (3.9 mmol) and 0.55 ml of Et3N were then added and, after about 5 minutes, a pH of 8-9 was adjusted by adding 0.5 ml of Et3N. The mixture was stirred at 0-4° C. for 1 hour and then at room temperature overnight. 50 ml of saturated NaHCO3 solution were then added to the mixture, and the organic phase was separated off. Drying and evaporating the solvent resulted in 620 mg of a reddish oil, which was reacted further immediately without further purification. The mixture was stirred at 0-4° C. for 1 hour at room temperature overnight the organic phase was separated off Drying evaporating the solvent
来源 ID: ord-6b46d268ecdb4ada8a7b6d15fb708a7b