反应详情

Dissolve 3-(3-bromo-6-chloro-2-fluoro-benzyl)-1-cyclohexyl-pyrrolidin-2-one (Example 30) (1 g, 2.6 mmol) and Pd(dppf)Cl2 (80 mg, 0.1 mol) in THF (degassed, 40 mL) and add 4-ethoxy-4-oxo-butylzinc bromide (15 mL, 7.7 mmol, 0.5 M THF solution). Reflux the reaction for 3 hours. Add the reaction mixture into ice and water. Extract the mixture with ethyl acetate (100 mL). Wash the organic layer with brine (50 mL), dry with magnesium sulfate, filter and evaporate solvent under reduced pressure. Purify the residue by column chromatography using 10% EA/H to 30% EA/H to obtain the title compound (1 g, 92%) as yellow oil: Mass spectrum (ion spray): m/z=424.1 (M+H).

1. temperatureReflux
2. customthe reaction for 3 hours
3. extractionExtract the mixture with ethyl acetate (100 mL)
4. washWash the organic layer with brine (50 mL)
5. dry with materialdry with magnesium sulfate
6. filtrationfilter
7. customevaporate solvent under reduced pressure
8. customPurify the residue by column chromatography