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Halogenated terephthalonitrile preparation method

A technology of terephthalonitrile and terephthaloyl chloride, which is applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high temperature, high pressure, and extremely high equipment requirements.

Inactive Publication Date: 2003-06-11
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Although this process method can carry out large-scale and continuous industrial production, because the ammoxidation method requires a fluidized bed, and the p-dibenzonitrile halogenation requires a tube reactor, and requires high temperature and high pressure, the requirements for equipment are extremely high. Therefore seek a kind of gentle, efficient, convenient, the preparation method of halogenated terephthalonitrile that is suitable for fine chemical industry is still the subject that people explore

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11

[0014] The preparation of embodiment 11. tetrachloroterephthalonitrile:

[0015] In a 1000 ml three-necked flask, 34 g of tetrachloroterephthaloyl chloride was dissolved in 600 ml of xylene, and then ammonia gas was introduced at 0°C, and a white solid was precipitated as the ammonia gas was introduced. Continue to feed ammonia, after about 10 liters, stop feeding ammonia. Raise the temperature to room temperature and continue stirring. After 4 hours, raise the temperature to 40°C to stop the reaction after removing unreacted ammonia gas from the system.

[0016] Add 15 milliliters of phosphorus oxychloride dropwise into the reaction flask, keeping the temperature below 60 degrees. After the dropwise addition was completed, the temperature was raised to 130° C. and refluxed for 6 hours. The reaction was stopped, the upper layer solution was separated, and the solvent was evaporated under reduced pressure to obtain 24 g of a white solid, with a yie...

Embodiment 22

[0018] Example 22. Preparation of tetrafluoroterephthalonitrile:

[0019] In a 1000 ml three-necked flask, dissolve 27.5 grams of tetrafluoroterephthaloyl dichloride in 500 ml of ethylene glycol dimethyl ether, and then start feeding ammonia gas at 0 degrees. With the feeding of ammonia gas, white solids are precipitated . Continue to feed ammonia, after about 10 liters, stop feeding ammonia. Raise the temperature to room temperature and continue stirring. After 4 hours, raise the temperature to 40°C to stop the reaction after removing unreacted ammonia gas from the system.

[0020] Add 15 milliliters of phosphorus oxychloride dropwise into the reaction flask, keeping the temperature below 60 degrees. After the dropwise addition was completed, the temperature was raised to 110° C. and refluxed for 5 hours. The reaction was stopped, the upper layer solution was separated, and the solvent was evaporated under reduced pressure to obtain 18.5 g of a w...

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Abstract

The invention is a method to prepare multi-halogen substituted terephthalonitrile. The halogen substituted terephthalyl chloride, molecular formula C1OC-C6HnX4-n-COCl, and liquid amine react to produce halogen substituted terephthalyl amine, then which forms the halogen substituted terephthalonitrile by dehydration. The above reaction can be one-step synthesized. In the formula, n=0.3, X=F, Cl or Br.

Description

technical field [0001] The invention relates to a preparation method of halogenated terephthalonitrile, in particular to a method for preparing halogenated terephthalonitrile in one step from halogenated terephthaloyl chloride. Background technique [0002] Halogenated terephthalonitriles include chlorinated terephthalonitriles, fluorinated terephthalonitriles and brominated terephthalonitriles, which are important dyes, pesticides and pharmaceutical intermediates, and have important applications in the chemical and pharmaceutical industries . And chlorinated terephthalonitrile is also an important raw material for preparing fluorinated terephthalonitrile. [0003] The current method for preparing halogenated terephthalonitriles in industry is to prepare p-dibenzonitriles (US patent 2,838,558, DE patent 954,241) by ammoxidation of p-xylene and then prepare chloro or brominated by chlorination or bromination. p-dibenzonitrile, finally fluorinated from chloro-p-dibenzonitril...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/00C07C253/22C07C255/51
Inventor 朱仕正赵经纬
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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