反应详情

6 mL Sulphuric acid is added to ‘2,2’-dithiodibenzoic acid (20 g, 65.3 mmol) in 150 mL methanol. The reaction mixture is refluxed 3 days. The reaction mixture is cooled to room temperature and saturated aqueous NaHCO3 is added. Methanol is removed in vacuo. The resulting heterogeneous mixture is extracted with ethyl acetate. The organic phase is washed with brine, dried with MgSO4 and concentrated in vacuo to give 17.8 g (82%) of the title compound as a solid, which is used without further purification.

1. temperatureThe reaction mixture is refluxed 3 days
2. customMethanol is removed in vacuo
3. extractionThe resulting heterogeneous mixture is extracted with ethyl acetate
4. washThe organic phase is washed with brine
5. dry with materialdried with MgSO4
6. concentrationconcentrated in vacuo