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Method for synthesizing thioanisole by using thiophenol and dimethyl carbonate as raw materials

A technology of dimethyl carbonate and thioanisole, applied in the field of synthesizing thioanisole, can solve problems such as pollution, and achieve the effects of avoiding environmental pollution, high yield and high product yield

Pending Publication Date: 2021-07-27
SHAANXI COAL & CHEM TECH INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the pollution problem existing in the existing thioanisole production technology, the purpose of the invention is to propose a method for synthesizing thioanisole with thiophenol and dimethyl carbonate as raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In mole percent, 65% of NaBr and MgBr 2 mixture and 35% Mn(NO 3 ) 2 and Fe(NO 3 ) 3 The mixture is mixed to obtain a composite catalyst.

[0027] In a 200ml miniature autoclave, add thiophenol and dimethyl carbonate with a molar ratio of 1:2, and add a composite catalyst whose mass is 1% of the mass of thiophenol, the stirring speed is 80r / min, and the reaction temperature is 130 °C, reaction pressure 6MPa, reaction time 6h in nitrogen atmosphere. After the reaction, the reaction liquid was detected by gas chromatography, the conversion rate of thiophenol was 78%, and the yield rate of thioanisole was 77%.

[0028] Wherein, the yield of thioanisole=the conversion rate of thiophenol*selectivity. The present invention provides a new and greener reaction system, and simultaneously provides a catalyst applied to the reaction system, under the action of the catalyst, the reactant thiophenol and dimethyl carbonate are directly reacted without additional introduction of ...

Embodiment 2

[0030] In mole percent, 70% LiBr and CaBr 2 mixture and 30% Zn(NO 3 ) 2 and Fe(NO 3 ) 3 The mixture is mixed to obtain a composite catalyst.

[0031] In a 200ml miniature autoclave, add thiophenol and dimethyl carbonate with a molar ratio of 1:1.2, and add a composite catalyst whose mass is 1% of the mass of thiophenol, the stirring speed is 100r / min, and the reaction temperature is 150 °C, reaction pressure 5MPa, reaction time 5h in nitrogen atmosphere. After the reaction, the reaction liquid was detected by gas chromatography, the conversion rate of thiophenol was 90%, and the yield rate of thioanisole was 85%.

Embodiment 3

[0033] In mole percent, 85% of NaBr and MgBr 2 mixture and 15% Mn(NO 3 ) 2 and Fe(NO 3 ) 3 The mixture is mixed to obtain a composite catalyst.

[0034] In a 200ml miniature autoclave, add thiophenol and dimethyl carbonate with a molar ratio of 1:1.5, and add a composite catalyst whose mass is 0.6% of thiophenol mass, the stirring speed is 150r / min, and the reaction temperature is 160 °C, reaction pressure 4MPa, reaction time 5h in nitrogen atmosphere. After the reaction, the reaction solution was detected by gas chromatography, the conversion rate of thiophenol was 100%, and the yield rate of thioanisole was 98%.

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Abstract

The invention discloses a method for synthesizing thioanisole by using thiophenol and dimethyl carbonate as raw materials. The method comprises the following steps: mixing thiophenol and dimethyl carbonate according to a molar ratio of 1: (1-2), adding a composite catalyst accounting for 0.1-5.0% of the weight of thiophenol, reacting for 1-8 hours in a nitrogen environment at 120-250 DEG C under the reaction pressure of 2-7MPa, stirring at the speed of 50-200r / min during the reaction, and after the reaction, distilling and purifying to obtain the thioanisole. The invention provides a novel greener reaction system and also provides a composite catalyst applied to the reaction system. The reactants thiophenol and dimethyl carbonate can directly react under the action of the composite catalyst, a water phase and a phase transfer accelerant are not required to be introduced, the reaction is simple, the reaction yield is high, almost no waste liquid is generated, and environmental pollution is avoided.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for synthesizing thioanisole with thiophenol and dimethyl carbonate as raw materials. Background technique [0002] Thioanisole, also known as thioanisole and methyl phenyl sulfide, is an important organic chemical raw material, which can be used as a raw material for drugs, pesticides, spices and photoinitiators, and can also be used as a stabilizer for vitamin A , Antioxidant of aromatic amine, lubricating additive, etc. [0003] At present, thioanisole is mainly produced by the methylation reaction of thiophenol. Commonly used methylating reagents are dimethyl sulfate, methyl iodide, and quaternary ammonium salts. Wherein the dimethyl sulfate route has a large amount of solid waste and high-salt, high chemical oxygen demand, highly toxic waste water to produce, and environmental pollution is serious; The route of methyl iodide has a large amount o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C321/28B01J27/25
CPCC07C319/14B01J27/25C07C321/28
Inventor 聂颖颖严良薛其才戚文博寇永利徐桥桥李蕾蕾许明杰
Owner SHAANXI COAL & CHEM TECH INST
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