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Synthetic method for preparing thiophenecarboxaldehyde

A technology of thiophene formaldehyde and synthesis method, which is applied in the direction of organic chemistry and the like, can solve the problems of low yield of thiophene formaldehyde, leakage of phosgene, insufficient purity, etc., and achieves the advantages of improving yield and purity, ensuring airtightness and simple operation. Effect

Inactive Publication Date: 2016-09-28
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the problems of low thiophene formaldehyde yield, insufficient purity, environmental pollution and easy leakage when using phosgene in the prior art, and to provide a synthetic method for preparing thiophene formaldehyde

Method used

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  • Synthetic method for preparing thiophenecarboxaldehyde
  • Synthetic method for preparing thiophenecarboxaldehyde

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Experimental program
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Effect test

Embodiment 1

[0020] A kind of synthetic method for preparing thiophene formaldehyde mainly comprises the following steps:

[0021] (1) Add 0.2mol DMF and 0.3mol solvent dichloroethane CH to the synthesizer 2 Cl 2 Finally, feed 0.1mol phosgene into the synthesizer through a feed pipe with a safety valve at the port and a seamless steel casing with an alarm on the side of the safety valve, and control the reaction temperature to 0°C. Generate the Vilsmeier-Haack reagent after the reaction;

[0022] (2) Add 0.5 mol of raw material thiophene dropwise to the Vilsmeier-Haack reagent at normal temperature, and control the reaction temperature to be 60° C.;

[0023] (3) After the reaction, first cool the product to room temperature, add process water to hydrolyze to obtain crude thiophene formaldehyde, after standing for stratification, extract the water layer with benzene and rectify to obtain pure thiophene formaldehyde, the tail gas after the reaction Can be absorbed by lye.

[0024] The yi...

Embodiment 2

[0026] A kind of synthetic method for preparing thiophene formaldehyde, its synthetic method comprises the following steps:

[0027] (1) Add 0.2mol DMF and 0.3mol solvent dichloroethane CH to the synthesizer 2 Cl 2 Finally, pass 0.1mol phosgene into the synthesizer through a seamless steel casing with a safety valve at the port and an alarm on the side of the safety valve, and control the reaction temperature to 0°C. Generate Vilsmeier-Haack reagent;

[0028] (2) Add 0.5 mol of raw material thiophene dropwise to the Vilsmeier-Haack reagent at normal temperature, and control the reaction temperature to be 30° C.;

[0029] (3) After reacting for a period of time, first cool the product to room temperature, add process water to hydrolyze to obtain crude thiophene formaldehyde, after standing for stratification, extract the water layer with benzene and rectify to obtain pure product thiophene formaldehyde, after the reaction ends Exhaust gas can be absorbed by lye.

[0030] Th...

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Abstract

The invention provides a kind of synthetic method for preparing thiophene formaldehyde, can be divided into three steps: (1) after adding N,N-dimethylformamide and solvent dichloroethane in the synthesizer, feed phosgene, Control the reaction temperature, generate Vilsmeier-Haack reagent after the end of the reaction; (2) drop raw material thiophene in the Vilsmeier-Haack reagent at normal temperature, control the reaction temperature; (3) After the reaction is over, first cool the product to room temperature, and then add The process water is hydrolyzed to obtain crude thiophene formaldehyde, and the pure product thiophene formaldehyde is obtained after layering, extraction and rectification; the preparation method of the present invention is simple, can effectively improve the yield and purity of the product, and avoids the leakage of phosgene and the passage of The alarm can promptly deal with possible toxic gas leakage.

Description

Technical field: [0001] The invention relates to a synthetic method for preparing thiophene formaldehyde, in particular to the field of organic synthesis. Background technique: [0002] Thiophene formaldehyde, also known as 2-thiophene formaldehyde, is slightly soluble in water and easily soluble in alcohol, benzene and ether. Thiophene formaldehyde is an important pharmaceutical intermediate, which is widely used as an intermediate of broad-spectrum anthelmintic drug pyrantel and drug cephalosporin 1 and 2. At present, the production capacity of thiophene formaldehyde in Chinese enterprises is small, so the market of thiophene formaldehyde is mainly abroad, and the domestic application is still in its infancy, which also restricts the expansion of production capacity and technological innovation of thiophene formaldehyde. [0003] The synthetic method of thiophene carboxaldehyde mainly contains at present: [0004] (1) Through thiophene, DMF and POCl 3 It is prepared by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/22
CPCC07D333/22
Inventor 黄金祥过学军吴建平胡明宏杨亚明程伟家李红卫徐小兵黄显超戴玉婷
Owner ANHUI GUANGXIN AGROCHEM
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