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A kind of method for preparing sulfoxide compound by photocatalytic oxidation of sulfide in aqueous phase

A technology of photocatalytic oxidation of thioether compounds, applied in the preparation of organic compounds, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as high toxicity, achieve high conversion rate, small impact, and mild reaction conditions Effect

Active Publication Date: 2022-06-24
NANYANG NORMAL UNIV
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Problems solved by technology

For example, Chinese patent document CN110194730A discloses a metal-organic framework material DUT-67(Zr) with photocatalytic oxidation of methyl phenyl sulfide. When it is used for photocatalytic oxidation of sulfide, the reaction system needs to use Methanol and trifluorotoluene are used as reaction solvents, which are highly toxic

Method used

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  • A kind of method for preparing sulfoxide compound by photocatalytic oxidation of sulfide in aqueous phase
  • A kind of method for preparing sulfoxide compound by photocatalytic oxidation of sulfide in aqueous phase
  • A kind of method for preparing sulfoxide compound by photocatalytic oxidation of sulfide in aqueous phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 Catalyst Bi 4 O 5 Br 2 preparation

[0020] 4 mmol KBr was dissolved in 40 mL of glycerol (solution A), 4 mmol of Bi (NO 3 ) 3 ·5H 2 O was dissolved in 40 mL of glycerol (solution B). Then, the above solution A was added dropwise to the solution B, and the mixture was uniformly mixed for about 30-60 minutes with continuous stirring. Then the uniformly mixed solution was transferred to the reaction kettle, placed in an oven at 160 ° C for 16 h, taken out from the reaction kettle, and then the upper layer of glycerol was poured out, and the lower layer of black matter was stirred with absolute ethanol and transferred to a centrifuge tube, centrifuged ( 1000 r / min, 2 min), the obtained solid was washed several times with absolute ethanol, and dried in an oven at 40° C. overnight to obtain a dry precursor. Put this precursor in a 500mL clean large beaker, add a large amount of deionized water, and continue stirring at 55 ° C for 48h, until the liquid and so...

Embodiment 2

[0021] Embodiment 2 The method for preparing sulfoxide compound by photocatalytic oxidation of sulfide in aqueous phase:

[0022] 20mg catalyst, 0.2mmol sulfide compound, 1mL water were added to 10mL two-necked flask successively, using O 2 Displacement for half an hour, followed by an atmosphere of O 2 Under protection, the reaction flask was irradiated with a 30W blue LED for 6-16 hours at room temperature. After the reaction, it was extracted with ethyl acetate solvent, the organic phase was dried and the conversion rate and selectivity were detected by gas chromatography (GC), and the product was qualitatively analyzed by gas chromatography-mass spectrometry (GC-MS).

Embodiment 3

[0023] Example 3 Photocatalytic oxidation of sulfide to synthesize sulfoxide compound (the catalyst used in this example was prepared according to the preparation method of Example 1)

[0024] 3.1 Photocatalytic oxidation of thioanisole: 20 mg of catalyst, 0.2 mmol of thioanisole, one atmosphere of O 2 Protected, stirred at room temperature, and irradiated the reaction flask with a 30W blue LED for 6 hours. The conversion rate was 99%, and the selectivity was 98%.

[0025]

[0026] 3.2 Photocatalytic oxidation of 2-methoxyanisole sulfide: 20 mg of catalyst, 0.2 mmol of 2-methoxyanisole sulfide, at atmospheric pressure O 2 Protected, stirred at room temperature, and irradiated the reaction flask with a 30W blue LED for 12 hours. The conversion rate was 99%, and the selectivity was 98%.

[0027]

[0028] 3.3 Photocatalytic oxidation of 4-methoxyanisole sulfide: 20 mg of catalyst, 0.2 mmol of 4-methoxyanisole sulfide, at atmospheric pressure O 2 Protected, stirred at ro...

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Abstract

The invention belongs to the technical field of synthesis of sulfoxide compounds, and in particular relates to a method for preparing sulfoxide compounds by photocatalytic oxidation of sulfide in water phase. In the present invention, a sulfide compound, a catalyst and water are placed in a reaction container, and the sulfoxide compound can be prepared by photocatalytic oxidation reaction at room temperature, blue light irradiation and the presence of oxygen; the catalyst is Bi 4 o 5 Br 2 . The method for preparing sulfoxide compounds by photocatalytically oxidizing sulfides in the aqueous phase is simple, environmentally friendly, has high conversion rate and good selectivity.

Description

technical field [0001] The invention belongs to the technical field of sulfoxide compound synthesis, in particular to a method for preparing a sulfoxide compound by photocatalytic oxidation of sulfide in an aqueous phase. Background technique [0002] Sulfoxide compounds are an important class of organic intermediate compounds, which can be widely used in chemistry, pharmacology, biology and other fields. Catalytic oxidation of sulfide compounds is a common method for the synthesis of sulfoxide compounds. In the reported catalytic systems, cheap and safe aqueous hydrogen peroxide solution is often used as the oxidant to oxidize sulfide to produce sulfoxide or sulfone. With the current in-depth research on energy development and solar energy utilization, photocatalysis as a new type of catalytic oxidation system has been gradually developed by everyone. In particular, the application of visible light in the field of organic synthesis has attracted the attention of many rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/02C07C317/14C07C317/22B01J27/06
CPCC07C315/02B01J27/06B01J35/004C07C317/14C07C317/22
Inventor 杨春霞赵伟
Owner NANYANG NORMAL UNIV
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