反应详情

Lithium hydroxide hydrate (6.44 ml, 232 mmol) was added to a stirred solution of tert-butyl 4-(4-chlorophenyl)-2,2-dimethyl-5-oxopyrrolidine-1-carboxylate (7.5 g, 23.2 mmol) in THF/MeOH/H2O (30 mL/30 mL/30 mL) at room temperature. The reaction mixture was stirred overnight and then concentrated in vacuo. The reaction mixture was taken up into water (200 mL), washed with EtOAc (100 mL), acidified with concentrated HCl and extracted into EtOAc (2×200 mL). The product was dried over Na2SO4 and concentrated in vacuo. The residual HCl was removed by evaporating from toluene to give 4-(tert-butoxycarbonylamino)-2-(4-chlorophenyl)-4-methylpentanoic acid (5.0 g, 63.2% yield) as a white solid. LCMS (APCI+) [M-Boc+H]+ 242.0; Rt: 2.8 min.

1. concentrationconcentrated in vacuo
2. washwashed with EtOAc (100 mL)
3. extractionextracted into EtOAc (2×200 mL)
4. dry with materialThe product was dried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residual HCl was removed
7. customby evaporating from toluene