反应详情

Precursors suitable for preparation of fullerene derivatives were prepared. First, methyl 4-benzoylbutyrate was prepared as follows. A solution of 4-benzoylbutyric acid (11.9 g, 0.0619 mol) in MeOH (250 ml) with a catalytic amount of sulfuric acid (96%, 6 drops) was refluxed for 5 hours. Solvent was removed and 50 ml water was added. The reaction product was extracted with dichloromethane to provide an organic layer. The organic layer was separated, dried over MgSO4 and passed through a plug of silica, which was rinsed with 2% acetone in dichloromethane. Solvent was removed to afford the methyl ester as light-yellowish oil (12.57 g, 99%).

1. customwere prepared
2. customSolvent was removed
3. addition50 ml water was added
4. extractionThe reaction product was extracted with dichloromethane
5. customto provide an organic layer
6. customThe organic layer was separated
7. dry with materialdried over MgSO4
8. washwas rinsed with 2% acetone in dichloromethane
9. customSolvent was removed