Method for preparing sulfone by catalytic oxidation of thioether

A technology for oxidizing sulfur and sulfide, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low conversion rate and high cost, and achieve the effects of easy separation, reduced pollution and high yield

Inactive Publication Date: 2004-11-17
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

As reported by Okun et al., iron-containing oxygen-containing clusters were immobilized on silica with positive ions (Okun, N.M.; Anderson, T.M.; Hill, C.L.J.Am.Chem.Soc.2003, 125, 3192-3193 .), due to the limitation of the oxidation performance of iron itself, the conversion rate is relatively low
Choudary et al. OsO 4 2- Negative ions were inserted into the interlayer of magnesium aluminum hydrotalcite (Choudary, B.M.; Reddy, C.R.V; Prakash, B.V; Kantam, M.L.; Sreedhar, B. Chem. Commun. 2003, 754-755.), the resulting LDH-OsO 4 The catalyst has high thioether catalytic performance, but the cost of the reaction is high

Method used

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  • Method for preparing sulfone by catalytic oxidation of thioether
  • Method for preparing sulfone by catalytic oxidation of thioether
  • Method for preparing sulfone by catalytic oxidation of thioether

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Experimental program
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Effect test

Embodiment 1

[0016] Catalyst preparation:

[0017] 14.4mmol FeCl 3 and 8.0 mmol MnCl 2 4H 2 O was dissolved in 20 mL deionized water, 0.4 mmol RuCl 3 and 1.2mmol Cu(NO 3 ) 2 The mixed aqueous solution was added to the above solution while stirring; the obtained mixed solution was slowly added to 40 mL of 124.2 mmol NaOH aqueous solution while stirring. After the addition, continue to stir the obtained slurry and raise the temperature to 110°C. After stirring for another 2 hours, stop stirring and let it cool naturally; After one hour, be cooled to room temperature, grind and promptly make 1.75g ​​black solid catalyst MnFe 1.8 Cu 0.15 Ru 0.05 o 4 .

Embodiment 2

[0019] Oxidation of sulfide anisole:

[0020] The oxidation reactions of sulfide anisole were carried out in glass tubes. The reaction tube is heated by an oil bath. 2mmol of sulfide anisole, 0.3g of MnFe 1.8 Cu 0.15 Ru 0.05 o 4 The catalyst and 5 mL of toluene solvent were mixed in the reaction tube in advance. Oxygen was provided by commercially available balloons filled with oxygen. The reaction products were detected by Shimadzu GC-14C gas chromatography, and naphthalene was used as an internal standard. The reaction temperature was 80°C. The reaction formula is as follows:

[0021]

[0022] After reacting for 12 hours under the above conditions, the conversion rate of sulfide anisole was 100%, and the selectivity of methyl phenyl sulfone was over 99%.

Embodiment 3

[0024] Oxidation of methyl phenyl sulfoxide:

[0025] The oxidation reactions of methyl phenyl sulfoxide were carried out in glass tubes. The reaction tube is heated by an oil bath. 2mmol of methyl phenyl sulfoxide, 0.3g of MnFe 1.8 Cu 0.15 Ru 0.05 o 4 The catalyst and 5 mL of toluene solvent were mixed in the reaction tube in advance. Oxygen was provided by commercially available balloons filled with oxygen. The reaction products were detected by Shimadzu GC-14C gas chromatography, and naphthalene was used as an internal standard. The reaction temperature was 60°C. The reaction formula is as follows:

[0026]

[0027] After reacting for 6 hours under the above conditions, the yield of the product methyl phenyl sulfone was over 99%.

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Abstract

The invention provides a process for preparing sulfur ether through catalytic oxidation comprising the steps of, adding 1-3 parts of raw material sulfur ether and 0.2-1 parts of solid catalyst MnFe[1,8]Cu[0.15]O4 into 5-10 parts of toluene solvent, reacting in oxygen atmosphere with a reaction temperature of 60-100 deg. C, wherein the parts of toluene solvent is by volume, the parts of sulfur ether is by mole parts, and the parts of catalyst is by weight. By using O2 as oxidizing agent for sulfur ether oxidization, the invention achieves the advantages of no environmental pollution and potential safety hazard proof.

Description

technical field [0001] The invention relates to a method for preparing sulfone by catalytically oxidizing sulfide, in particular to a method for preparing sulfone by oxidizing sulfide under mild conditions by using only oxygen as an oxidant and using a recyclable and reusable catalyst. Background technique [0002] Sulfoxides and sulfones are important chemicals widely used in pharmaceuticals and chemical intermediates. Due to the requirements of environmental friendliness, the oxidation of sulfides and sulfoxides has been developed from the use of metered oxidants to catalytic oxidation, from organic or inorganic salt oxidants that are expensive and may cause subsequent treatment difficulties or environmental pollution to oxygen and hydrogen peroxide. , from the homogeneous catalysis that is difficult to recycle after the reaction to the reusable solid-phase catalyst. In the reported research, there are not many liquid-solid phase catalytic reaction systems using oxygen as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/02
Inventor 纪红兵钱宇罗思睿
Owner SOUTH CHINA UNIV OF TECH
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