反应详情

温度

65 °C

Potassium trimethylsilanolate (0.090 g) was added to a solution of N-(1,1′-biphenyl-4-yl)-N′-(3-{[2-({6-[(5R)-5-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo-1,3-oxazolidin-3-yl]hexyl}oxy)ethoxy]methyl}phenyl)urea (0.119 g) in deoxygenated anhydrous THF (4 ml) whilst stirring under nitrogen. The reaction mixture was heated to 65° C. for 3 h, at which point the reaction mixture was cooled to room temperature. Phosphate buffer (25 ml, pH6.5) was added and the mixture extracted with EtOAc (3×25 ml). The combined organic layers were separated and dried over Na2SO4 before filtering. Solvent evaporation in vacuo gave a residue which was purified by Biotage. Elution with 150:8:1 dichloromethane:EtOH:ammonia followed by solvent evaporation in vacuo gave the title compound (0.092 g). LCMS RT=3.16 min, ES+ve 668 (MH)+.

1. temperaturewas cooled to room temperature
2. extractionthe mixture extracted with EtOAc (3×25 ml)
3. customThe combined organic layers were separated
4. dry with materialdried over Na2SO4
5. filtrationbefore filtering
6. customSolvent evaporation in vacuo
7. customgave a residue which
8. customwas purified by Biotage
9. washElution with 150:8:1 dichloromethane
10. customEtOH:ammonia followed by solvent evaporation in vacuo