反应详情

A mixture of 2-benzoyloxyacetaldehyde (example (5.65 g), 1,2-ethanedithiol (3 ml) and paratoluenesulfonic acid (200 mg) in toluene (250 ml) was heated at refluxing under water removal conditions using a Dean Stark apparatus for 4 hours. The mixture was cooled to room temperature, washed first with saturated aqueous NaHCO3 solution (1×60 ml), then with water (2×60 ml), and dried over reduced pressure. The residue was purified by chromatography on silica gel using hexane:ethyl acetate (9:1) as eluant to give 5.2 g of pure product which was characterized by 1H- and 13C-NMR spectroscopy.

1. temperaturewas heated
2. temperatureat refluxing under water
3. customremoval conditions
4. customfor 4 hours
5. washwashed first with saturated aqueous NaHCO3 solution (1×60 ml)
6. dry with materialwith water (2×60 ml), and dried over reduced pressure
7. customThe residue was purified by chromatography on silica gel