反应详情

A mixture of methyl 4′-[((4,4-dimethylcyclohexyl){[(1,1-dimethylethyl)oxy]carbonyl}-amino)methyl]-3-biphenylcarboxylate (0.850 g; 1.88 mmol), LiOH.H2O (0.395 g; 9.40 mmol), water (2 mL) and THF (20 mL) was heated under reflux for 24 h, cooled and concentrated in vacuo. The residue was partitioned between EtOAc/1N KHSO4, layers were separated and the organic layer was extracted with EtOAc (×2). combined organics were washed (water, brine), dried over Na2SO4 and concentrated in vacuo affording the title compound as a colorless foam. LC/MS (method E) tR 0.77 min; m/z 464 (M−H).

1. temperaturewas heated
2. temperatureunder reflux for 24 h
3. temperaturecooled
4. concentrationconcentrated in vacuo
5. customThe residue was partitioned between EtOAc/1N KHSO4, layers
6. customwere separated
7. extractionthe organic layer was extracted with EtOAc (×2)
8. washcombined organics were washed (water, brine)
9. dry with materialdried over Na2SO4
10. concentrationconcentrated in vacuo