反应详情

To a solution of [3-(4′-formyl-3-biphenylyl)-1H-pyrazol-1-yl]methyl 2,2-dimethyl-propanoate (0.162 g; 0.45 mmol) in 1:1 THF/MeOH (5 mL total vol) at room temperature was added NaOH (1.1 mL of a 1.0M solution; 1.1 mmol). After 30 min, HOAc (0.08 mL; 1.4 mmol) was added and the mixture was concentrated in vacuo. The residue was partitioned between EtOAc/water, layers were separated, the organic layer was washed (satd NaHCO3, brine), dried over Na2SO4 and concentrated in vacuo. The residue was redissolved in EtOAc, washed (1M HCl, water, brine), dried over Na2SO4 and concentrated in vacuo, affording the title compound as a glassy semi-solid which was used without further purification. LC/MS (method A) 2.42 min; m/z 249 (M+H).

1. concentrationthe mixture was concentrated in vacuo
2. customThe residue was partitioned between EtOAc/water, layers
3. customwere separated
4. washthe organic layer was washed (satd NaHCO3, brine)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. dissolutionThe residue was redissolved in EtOAc
8. washwashed (1M HCl, water, brine)
9. dry with materialdried over Na2SO4
10. concentrationconcentrated in vacuo