Method for synthesizing sulfone compounds under photocatalytic conditions
A compound and photocatalytic technology, which is applied in the preparation of organic compounds, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., and can solve the problems of harsh reaction conditions and limited substrate universality. , to achieve the effect of easy operation, widening new applications and low price
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Embodiment 1
[0039] Example 1 Preparation of diphenyl sulfone
[0040] With a quartz reaction tube, a magnetic stirreon was added thereto, then 0.3 mmol of benzide, 0.9 mmol of benzenesulfonate, 0.9 mmol of cesium carbonate (CS)2 CO 3 ), 5 mmol% of photosensitizer polyate ([N-bu " 4 ) N] 4 [W 10 O 32 ], TBADT), and finally add 1 ml of dimethyl sulfoxide (DMSO).
[0041] Then, a three-way director head with a balloon is added above the quartz reaction tube, first with liquid nitrogen to freeze the reactant liquid, then remove the quartz reaction tube to the quartz reaction tube, then charge the balloon full of oxygen; magnetic stirrer stir Next, the reaction was irradiated under the oxygen conditions for 12 h, and the final product was detected by TLC, and finally the final product diphenyl sulfoxide was separated by column chromatography, and the yield was 58%.
[0042] The reaction equation is as follows:
[0043]
[0044] The nuclear magnetic resonance spectrum of di苯 sulfone is as follows...
Embodiment 2
[0046] Example 2 4-Preparation of methyl diphenyl sulfone
[0047] With a stone reaction tube, a magnetic stirreon was added thereto, then 0.3 mmol of 4-methylbenzine, 0.9 mmol of benzulla sodium, 0.9 mmol of cesium carbonate (CS) 2 CO 3 5 mmol% of the photosensitizer Eosin Y, finally added dimethyl sulfoxide (DMSO) 1 ml.
[0048] Then, a three-way director head with a balloon is added above the quartz reaction tube, first with liquid nitrogen to freeze the reactant liquid, then remove the quartz reaction tube to the quartz reaction tube, then charge the balloon full of oxygen; magnetic stirrer stir Next, the reaction was irradiated under the oxygen conditions for 12 h, and the final product was detected by TLC, and finally the final product 4-methyl diphenyl sulfone was separated by column chromatography, and the yield was 52%.
[0049] The reaction equation is as follows:
[0050]
[0051] The 4-methyl dithyloxide nuclear magnetic resonance spectrometry is as follows: 1 H NMR ...
Embodiment 3
[0052] Example 3 Preparation of 4-cyano-cyannyl dithiasis
[0053] With a quartz reaction tube, a magnetic stirreon was added thereto, then 0.3 mmol of 4-cyanobenzide, 0.9 mmol of benzulse sodium, 0.9 mmol of cesium carbonate (CS) 2 CO 3 ), 15mmol% of photosensitizer polyate ([N-bu " 4 ) N] 4 [W 10 O 32 ], TBADT), and finally add 1 ml of dimethyl sulfoxide (DMSO).
[0054] Then, a three-way director head with a balloon is added above the quartz reaction tube, first with liquid nitrogen to freeze the reactant liquid, then remove the quartz reaction tube to the quartz reaction tube, then charge the balloon full of oxygen; magnetic stirrer stir Next, the reaction was irradiated under oxygen conditions under the oxygen conditions for 12 h, and the final product was detected by TLC, and finally the final product 4-cyanobenyl sulfone was separated by column chromatography, and the yield was 87%.
[0055] The reaction equation is as follows:
[0056]
[0057] The nuclear magnetic reson...
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