反应详情

To 20 ml of ethanol were added 1.37 g of p-hydroxy-6-(1-imidazolyl)hexaneanilide and 0.69 g of anhydrous potassium carbonate and the mixture was stirred for 30 minutes with heating under reflux. After cooling, 1.26 g of ethyl 6-bromo-2,2-dimethylhexanoate was added thereto and the mixture was reacted overnight with heating under reflux. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the resulting residue followed by extracting with chloroform. After the chloroform layer was successively washed with a 1N aqueous sodium hydroxide solution and a saturated aqueous sodium chloride solution, it was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure and the resulting residue was subjected to silica gel column chromatography. The product was eluted out using a chloroform-methanol liquid mixture (50:1 in a volume ratio). The solvent was removed by distillation under reduced pressure. The resulting crystals were recrystallized from a solvent mixture of n-hexane-ethylacetate to obtain ethyl 6-[p-[6-(1-imidazolyl)hexanamido]phenoxy]-2,2-dimethylhexanoate as white crystals.

1. temperaturewith heating
2. temperatureunder reflux
3. temperatureAfter cooling
4. customthe mixture was reacted overnight
5. temperaturewith heating
6. temperatureunder reflux
7. customThe solvent was removed from the reaction mixture by distillation under reduced pressure
8. additionWater was added to the resulting residue
9. extractionby extracting with chloroform
10. washAfter the chloroform layer was successively washed with a 1N aqueous sodium hydroxide solution
11. dry with materiala saturated aqueous sodium chloride solution, it was dried over anhydrous magnesium sulfate
12. customThe solvent was removed by distillation under reduced pressure
13. washThe product was eluted out
14. customThe solvent was removed by distillation under reduced pressure
15. customThe resulting crystals were recrystallized from a solvent mixture of n-hexane-ethylacetate