反应详情

To a solution of sodium iodide (2.80 g, 18.9 mmol) in acetone (20 mL) was added a solution of 3,3-diphenylpropyl methanesulfonate (5.00 g, 17.2 mmol) in acetone (10 mL) at 0° C. and the mixture was refluxed for 3 hours. After cooling, the solvent was distilled off under reduced pressure and the residue was diluted with water (30 mL) and extracted with 2 portions of ethyl acetate. The pooled extract was washed with saturated aqueous sodium chloride solution, dried over MgSO4, and filtered. The filtrate was concentrated under reduced pressure and the residue was crystallized from methanol to provide 4.70 g of the title compound. Yield 85%.

1. temperaturethe mixture was refluxed for 3 hours
2. temperatureAfter cooling
3. distillationthe solvent was distilled off under reduced pressure
4. additionthe residue was diluted with water (30 mL)
5. extractionextracted with 2 portions of ethyl acetate
6. extractionThe pooled extract
7. washwas washed with saturated aqueous sodium chloride solution
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationThe filtrate was concentrated under reduced pressure
11. customthe residue was crystallized from methanol