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Industrial prepn process of tetrachloro terephthalonitrile

A technology of tetrachloroterephthalonitrile and tetrachloroterephthalic acid, applied in the dehydration preparation of carboxylic acid amide, organic chemistry, etc., to achieve the effect of simple process

Inactive Publication Date: 2006-08-02
魏晓廷
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Problems solved by technology

As verified by the Jiangsu Science and Technology Novelty Search Consulting Center (report number 200632B2500553), there is no domestic supply of this product, and no report on the preparation method of this product

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  • Industrial prepn process of tetrachloro terephthalonitrile
  • Industrial prepn process of tetrachloro terephthalonitrile
  • Industrial prepn process of tetrachloro terephthalonitrile

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Embodiment

[0021] Step 1: the preparation of tetrachloroterephthalic acid, in 1000ml flask, add 1mol terephthalic acid, 1g iodine, add the concentrated sulfuric acid that 500ml concentration is 40%~50%, pass into 4.5mol chlorine gas under the dark condition, The temperature is controlled between 80°C and 90°C, and a small amount of sulfuric acid is added in the later stage. When the temperature rises to 130°C, the ventilation speed should be slow and uniform. Slowly pour it into ice water, filter under ice water temperature to obtain a white solid, which is dried and crushed into powder, which is tetrachloroterephthalic acid;

[0022] Step 2: prepare tetrachloroterephthaloyl dichloride, put the tetrachloroterephthalic acid obtained in the previous step into a 2000ml flask, add 1200ml toluene and 2.2mol alumite chloride and 5mlDMF, slowly heat to reflux state, and keep warm for 6 Cool down after 1 hour, filter out impurities with absorbent cotton, remove the solvent, and cool down after r...

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Abstract

The present invention discloses industrial preparation process of tetrachloro terephthalonitrile. Tetrachloro terephthalonitrile is prepared with terephthalic acid as initial material and through four reaction steps, including the first step of chlorinating terephthalic acid to prepare tetrachloro terephthalic acid, the second step of preparing tetrachloro terephthalyl chloride; the third step of preparing tetrachloro terephthalyl amide; and the fourth step of preparing tetrachloro terephthalonitrile. The present invention has simple technological process, is suitable for match production and has product purity up to 99 % and product yield up to 70 %.

Description

Technical field: [0001] The present invention relates to the industrial preparation method of tetrachloroterephthalonitrile. Background technique: [0002] Tetrachloroterephthalonitrile is an off-white solid with the molecular formula C 8 N 2 Cl 4 , molecular weight: 266, structural formula: [0003] [0004] Tetrachloroterephthalonitrile is the key intermediate for the preparation of 2,3,5,6-tetrafluorobenzyl alcohol and 2,3,5,6-tetrafluoro-4-methylbenzyl alcohol, because 2,3,5 , 6-tetrafluorobenzyl alcohol is an intermediate in the synthesis of sanitation pyrethroid transfluthrin, which is a broad-spectrum insecticide and has good development prospects. 2,3,5,6-tetrafluoro-4-methylbenzyl alcohol is an intermediate in the synthesis of pyrethroids tefluthrin and profluthrin, both of which are promising pyrethroids. Pyrethrin products. Tetrachloroterephthalonitrile is the key intermediate for the synthesis of the above pyrethroids. As verified by the Jiangsu Science...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C255/51
Inventor 魏晓廷朱金玉
Owner 魏晓廷
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