Synthetic method of diaryl thioether
A technology of diaryl sulfide and synthesis method, which is applied in sulfide preparation, organic chemistry, etc., can solve the problems of increased reaction cost and troublesome post-processing, and achieves the effect of simple and easy operation of reaction steps, single product and high purity
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Embodiment 1
[0049] Synthesis of Diphenyl Sulfide
[0050] Add 0.6120 g (3 mmol) of iodobenzene into a 50 mL round bottom flask equipped with a stirring bar, then add the solvent dimethyl sulfoxide, and continue to add 0.0192 g (0.3 mmol) of Cu and 0.1368 g (1.8 mmol) of thiourea under stirring. mmol), KOH (content 82%) 0.4100 g (6.0 mmol), first stirred at room temperature for 15 min, heated to 130 °C and stirred for 36 hours. TLC tracking detection reaction, stop heating when the substrate is completely reacted or no longer reduced, add a mixture of ethyl acetate and water with a volume ratio of 1:1 to the system when the temperature drops to room temperature, filter to remove the solid in the system, and separate the liquid , the aqueous phase was extracted with ethyl acetate, and the resulting organic phases were combined, dried with magnesium sulfate, and purified by column chromatography [silica gel, 200-300 mesh; petroleum ether] to obtain a colorless liquid with a yield of 85%.
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Embodiment 2
[0054] Synthesis of Diphenyl Sulfide
[0055] Add 0.6120 g (3 mmol) of iodobenzene into a 50 mL round bottom flask equipped with a stirring bar, then add the solvent dimethyl sulfoxide, and continue to add 0.0192 g (0.3 mmol) of Cu and 0.1140 g (1.5 mmol) of thiourea under stirring. mmol), KOH (content 82%) 0.4100 g (6.0 mmol), first stirred at room temperature for 15 min, heated to 125 °C and stirred for 36 hours. TLC tracking detection reaction, stop heating when the substrate is completely reacted or no longer reduced, add a mixture of ethyl acetate and water with a volume ratio of 1:1 to the system when the temperature drops to room temperature, filter to remove the solid in the system, and separate the liquid , the aqueous phase was extracted with ethyl acetate, the resulting organic phases were combined, dried with magnesium sulfate, and purified by column chromatography [silica gel, 200-300 mesh; petroleum ether] to obtain a colorless liquid with a yield of 82%.
[005...
Embodiment 3
[0058] Synthesis of diphenyl sulfide The molar ratio of halogenated aromatic hydrocarbons, thiourea and potassium hydroxide is 5: 2.5-3: 5-10. The elemental copper powder is 8-15mol% of the halogenated aromatic hydrocarbons,
[0059] Add 0.6120 g (3 mmol) of iodobenzene into a 50 mL round bottom flask equipped with a stirring bar, then add the solvent dimethyl sulfoxide, and continue to add 0.0192 g (0.3 mmol) of Cu and 0.1368 g (1.8 mmol) of thiourea under stirring. mmol), KOH (content 82%) 0.2100 g (3.0 mmol), first stirred at room temperature for 15 min, heated to 130°C and stirred for 30 hours. TLC tracking detection reaction, stop heating when the substrate is completely reacted or no longer reduced, add a mixture of ethyl acetate and water with a volume ratio of 1:1 to the system when the temperature drops to room temperature, filter to remove the solid in the system, and separate the liquid , the aqueous phase was extracted with ethyl acetate, the resulting organic phas...
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