反应详情

4,4-Dimethyl-3-oxopentanenitrile (293 mg, 2.34 mmol) and Intermediate 67b (593 mg, 2.34 mmol) were suspended in MeOH (10 mL) and a few drops of concentrated HCl added and the reaction heated to reflux for 72 h. The reaction was cooled, concentrated in vacuo and partitioned between H2O and EtOAc. The organic layer was separated, and the aqueous extracted again with EtOAc. The combined organics were dried over MgSO4 and subjected to FCC, eluting with 10-50% EtOAc/cyclohexane to afford the title compound after crystallisation (139 mg, 21%). LCMS (Method 3) Rt 2.77 min, m/z 277.3 [MH+].

1. temperaturethe reaction heated
2. temperatureto reflux for 72 h
3. temperatureThe reaction was cooled
4. concentrationconcentrated in vacuo
5. custompartitioned between H2O and EtOAc
6. customThe organic layer was separated
7. extractionthe aqueous extracted again with EtOAc
8. dry with materialThe combined organics were dried over MgSO4
9. washeluting with 10-50% EtOAc/cyclohexane