反应详情

In 50 ml of ethanol was suspended 3 g of 4'-hydroxy-6-(1-imidazolyl)hexaneanilide hydrochloride. While stirring 2.8 g of anhydrous potassium carbonate and 2.4 g of ethyl 5-bromo-2,2-dimethylpentanoate were added to the suspension. The mixture was stirred for 8 hours under reflux. The solvent was removed from the reaction mixture by distillation under reduced pressure and the residue was dissolved in ethylene chloride. The solution was successively washed with a 5% aqueous hydrogen sodium carbonate solution, water and a saturated aqueous sodium chloride solution and then dried over anhydrous sodium sulfate. After drying, the solvent was removed by distillation under reduced pressure. The resulting crystals were recrystallized from ethyl acetate to give the aimed product, ethyl 5-[p-[6-(1-imidazolyl)hexanamido]phenoxy]-2,2-dimethylpentanoate.

1. additionwere added to the suspension
2. temperatureunder reflux
3. customThe solvent was removed from the reaction mixture by distillation under reduced pressure
4. dissolutionthe residue was dissolved in ethylene chloride
5. washThe solution was successively washed with a 5% aqueous hydrogen sodium carbonate solution, water
6. dry with materiala saturated aqueous sodium chloride solution and then dried over anhydrous sodium sulfate
7. customAfter drying
8. customthe solvent was removed by distillation under reduced pressure
9. customThe resulting crystals were recrystallized from ethyl acetate