反应详情

A mixture of 5 g of 2,2-dimethyllauric acid, 4.72 ml of diphenylphosphorylazide (DPPA), 3.36 ml of triethylamine and 80 ml of benzene was refluxed for one hour. After cooling, a mixed solution of 5.763 g of (2-amino-4-methoxy-6-tert-butylphenoxy)methoxymethane and 20 ml of benzene was added dropwise to the above mixture. The resulting mixture was stirred at room temperature for one hour and then under reflux for 10 hours. Water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate. The extract was washed and dried, and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (solvent; hexane:ethyl acetate=4:1) and the product was recrystallized from hexane to give 2.89 g of {2-[3-(1,1-dimethylundecyl)ureido]-4-methoxy-6-tert-butylphenoxy}methoxymethane (melting point: 83°-85° C.).

1. temperaturewas refluxed for one hour
2. temperatureAfter cooling
3. temperatureunder reflux for 10 hours
4. extractionthe reaction mixture was extracted with ethyl acetate
5. washThe extract was washed
6. customdried
7. customthe solvent was removed under reduced pressure
8. customThe residue was purified by silica gel column chromatography (solvent; hexane:ethyl acetate=4:1)
9. customthe product was recrystallized from hexane