反应详情

3,4-dimethoxyphenylsulfonyl chloride (2.3 mmol) was dissolved in acetone (60 mL), and then NaI (3.4 g, 23 mmol) and fluoroacetic anhydride (1.45 mL, 6.9 mmol) were added and the mixture was stirred at room temperature for one hour. The reaction solution was concentrated, water was added, extraction was performed with ether and the organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline. After drying over magnesium sulfate and vacuum concentration, the residue was purified with a silica gel column (hexane) to obtain 3,4-dimethoxyphenyldisulfide as a light yellow crystalline compound (58% yield). The NMR and mass spectral data for the obtained compound were as follows:

1. concentrationThe reaction solution was concentrated
2. additionwater was added
3. extractionextraction
4. washthe organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline
5. dry with materialAfter drying over magnesium sulfate and vacuum concentration
6. customthe residue was purified with a silica gel column (hexane)