反应详情

Add hydrazine hydrate (0.189 mL, 3.913 mmol) to a stirred suspension of 2-[4-(3,3-dimethyl-butyryl)-benzyl]-isoindole-1,3-dione (875 mg, 2.609 mmol) in methanol (15 mL). Heat the mixture to reflux overnight. Cool the mixture to room temperature and concentrate in vacuo. Partition the residue between EtOAc and 5N aqueous HCl and wash the acidic aqueous phase again with 5N aqueous HCl. Basify with 5N aqueous NaOH to pH 12. Extract the basic aqueous solution three times with chloroform. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to give the title compound as a yellow oil (411 mg, 77%) that was used without any further purification.

1. temperatureHeat the mixture
2. temperatureto reflux overnight
3. concentrationconcentrate in vacuo
4. customPartition the residue between EtOAc and 5N aqueous HCl
5. washwash the acidic aqueous phase again with 5N aqueous HCl
6. extractionExtract the basic aqueous solution three times with chloroform
7. dry with materialDry the combined organic extracts over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo