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A kind of preparation method of o-chlorobenzonitrile

A technology of o-chlorobenzonitrile and o-chlorobenzoic acid, which is applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problem of high price of o-chlorobenzaldoxime, affecting yield and product quality, The effect is not very ideal and other problems, to achieve the effect of avoiding complicated process equipment, stable product quality and low pollution

Active Publication Date: 2022-06-07
三门峡环宇生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wastewater treatment is difficult and costly
[0018] Some of the above-mentioned various preparation methods have defects such as low conversion rate, some raw materials are expensive and difficult to obtain, high toxicity, serious waste pollution, easy blockage of the reaction process, difficult operation and other defects, and the effect is not very satisfactory.
[0019] Among the above-mentioned methods, the first and fourth methods are the simplest and are prepared in one step, but the first raw material o-chlorobenzaldoxime is expensive and difficult to purchase in large quantities, and the raw material dehydrating agent amino group used in the preparation method of o-chlorobenzoic acid Sulfonic acid produces a large amount of waste residue, which affects the yield and product quality, and brings environmental protection treatment problems

Method used

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  • A kind of preparation method of o-chlorobenzonitrile
  • A kind of preparation method of o-chlorobenzonitrile
  • A kind of preparation method of o-chlorobenzonitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0038] To the 500ml four-necked flask equipped with a thermometer and a distillation column, add 160 g of o-chlorobenzoic acid with a content of 98.0%, 61 g of urea with a mass fraction of 46.3% total nitrogen (N) content, turn on the heating mantle power supply and heat up, when

[0039] When the temperature rises to 145°C, the melting is basically completed, and the stirring is turned on. The initial reaction is controlled at 140-180°C, and the reaction is performed for 4 h. The molar ratio of o-chlorobenzoic acid to urea was 1:1. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography, which was 81.2%. Ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.

[0040] Slowly heat up, react at 230~250°C for 1.5 h, then continue to raise the temperature at 250~270°C, react for 1.5 h, distill out the crude nitrile under reduced pressure, and the residue after...

Embodiment 2

[0044] Into the 500ml four-necked flask equipped with a thermometer and a distillation column, add 160 g of o-chlorobenzoic acid with a content of 98.0%, and 85 g of urea with a mass fraction of 46.0% total nitrogen (N) content, turn on the heating mantle power supply to heat up, when When the temperature rises to 145°C, the melting is basically completed, and the stirring is turned on. The initial reaction is controlled at 140-180°C, and the reaction is performed for 4 h. The molar ratio of o-chlorobenzoic acid to urea was 1:1.4. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography (89.1%). Ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.

[0045] Slowly heat up, react at 230~250°C for 1.5 h, then continue to heat up at 250~270°C, react for 1.5 h, distill out the crude nitrile under reduced pressure, and the residue after distillation contains the ...

Embodiment 3

[0049] Into the 500ml four-necked flask equipped with a thermometer and a distillation column, add 160 g of o-chlorobenzoic acid with a content of 98.0%, and 85 g of urea with a mass fraction of 46.4% total nitrogen (N) content, turn on the heating mantle power supply to heat up, and when When the temperature rises to 145°C, the melting is basically completed, the stirring is turned on, the reaction temperature is controlled at 140-180°C, and the reaction is carried out for 2 h. The content of o-chlorobenzamide in the reactant was detected by high performance liquid chromatography (88.3%). Ammonia and carbon dioxide released during the reaction are absorbed by water to generate ammonium bicarbonate aqueous solution.

[0050] Slowly heat up, the temperature is at 230~250 °C for 4 h, and then the temperature is controlled at 250~270 °C for 3 h, and the crude nitrile is distilled off under reduced pressure. The residue after distillation contains the intermediate produced by the ...

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Abstract

A preparation method of o-chlorobenzonitrile, which uses o-chlorobenzoic acid and urea as raw materials, the reaction is continuous and controllable, the product yield is well guaranteed and controllable, the reaction conditions are easy to control, the product quality is stable, and unreacted Raw materials and intermediate products can be recycled after recovery. Especially after the reaction of o-chlorobenzoic acid and urea to form o-chlorobenzamide, ultrasonic or microwave catalyzed high-temperature dehydration into o-chlorobenzonitrile, the yield is as high as 92%, and the product purity can reach 97%. Not only is the whole reaction process safe and clean, and the environmental protection treatment is easy, but it can also reduce the production wastewater of o-chlorobenzonitrile and realize the clean production of o-chlorobenzonitrile. The unreacted raw material o-chlorobenzoic acid and intermediates can be recycled after recycling can significantly reduce production costs. Moreover, it can avoid the disadvantages of complex equipment, high operation requirements, and low product yield in the traditional process, and has the characteristics of less "three wastes" and less pollution. It is another ideal way to realize industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of organic fine chemicals, especially a kind of preparation method of o-chlorobenzonitrile. It belongs to the technical field of organic chemistry, and also belongs to the technical field of organic fine chemicals. Background technique [0002] o-Chlorobenzonitrile (OCBN), also known as o-chlorobenzonitrile, is an important fine chemical and organic preparation intermediate. Using o-chlorobenzonitrile as raw material, the corresponding o-chlorobenzylamine, o-chloroaniline, o-fluorobenzonitrile, o-fluorobenzoic acid, o-fluoroaniline, etc. can be prepared, which are widely used in dyes, medicines, pesticides and fragrances and other industries. It is an important intermediate for the preparation of new antimalarial drug nitroquine, antihypertensive drug valsartan, uracil herbicides and phenylbenzamide insecticides. 2-Cyano-4-nitroaniline, an important intermediate of multi-purpose azo disper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/20C07C255/50C07C253/34
CPCC07C231/10C07C253/20C07C253/34C07C233/65C07C255/50
Inventor 张卫民梁振贤魏战勇谭静段敬杰张坤王馨悦王艳王志全
Owner 三门峡环宇生化科技有限公司