Sample method for synthesis of thianthrene based on sulfur powder
A technology of thianthrene and sulfur powder, which is applied in the field of environmentally friendly synthesis of thianthrene, achieving the effect of mild conditions and simple reaction operation
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[0009] The present invention is achieved in that in a 25 mL round bottom flask, add o-diiodobenzene (0.5 mmol), sulfur powder (0.5 mmol), cuprous iodide (0.05 mmol), 1,10-phenanthroline (0.1 mmol), potassium carbonate (1.0 mmol) and dimethyl sulfoxide (2 mL). The resulting mixed system is then 90 o C was stirred for 12 hours. After cooling to room temperature, 10 mL of water was added to the system, then extracted with ethyl acetate (3×10 mL), and dried over anhydrous sodium sulfate. After distilling off the solvent, the obtained residue was subjected to silica gel column chromatography to obtain a pure product with a yield of 82%. The reaction formula and data are as follows figure 1 shown. The structure and purity of the obtained product were determined by proton nuclear magnetic resonance spectrum and carbon spectrum test and compared with literature data.
[0010] The proton nuclear magnetic resonance spectrum and carbon spectrum data of product thianthrene are:
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