Synthesis method of benzoyl cyanide

A synthesis method, the technology of benzoyl cyanide, applied in the field of synthesis of benzoyl cyanide, can solve the problems of low conversion rate, high risk, difficult operation, etc., and achieve the effect of high conversion rate, simple operation and pollution reduction

Inactive Publication Date: 2019-04-19
江苏佳麦化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is in order to solve the shortcoming that exists in the prior art, as: the traditional technique has the problem of heavy metal pollution, simultaneously because temperature and time demand are higher, so caused conversion rate low, and benzoyl cyanide and benzoyl Acid anhydrides are difficult to separate, and the dimethylamine-catalyzed hydrocyanic acid method requires the use of highly toxic hydrocyanic acid, which is difficult and dangerous to operate

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  • Synthesis method of benzoyl cyanide

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Effect test

Embodiment 1

[0014] The synthetic method of embodiment one benzoyl cyanide

[0015] Put 100mL of toluene, 23.7g of 97% solid sodium cyanide, 0.06g of polyethylene glycol 600, 0.06g of trioctylmethylammonium chloride, and 0.1g of water into a 250mL four-necked flask, turn on the tail gas absorption device, stir, Circulating cooling water. Turn on the heating device and start heating. When the temperature of the reaction solution rose to 60°C, the cock of the constant pressure dropping funnel was opened, and 57.4g of benzoyl chloride was added dropwise, keeping the reaction temperature between 60°C and 85°C. The benzoyl chloride was dropped in about 1.5 hours. After the dropwise addition, the reflux reaction was continued and samples were taken to track the reaction process. When the mass fraction of benzoyl chloride in the reaction solution was less than 0.1%, the reaction was over, and it took about 4 hours. After cooling down to 35°C-45°C, filter, wash the filter residue twice with 40mL...

Embodiment 2

[0017] The synthetic method of embodiment dibenzoyl cyanide

[0018] Put 100mL of toluene, 23.7g of 97% solid sodium cyanide, 0.3g of polyethylene glycol 600, 0.3g of trioctylmethylammonium chloride, and 0.6g of water into a 250mL four-necked flask, turn on the tail gas absorption device, stir, Circulating cooling water. Turn on the heating device and start heating. When the temperature of the reaction solution rose to 60°C, the cock of the constant pressure dropping funnel was opened, and 57.4g of benzoyl chloride was added dropwise, keeping the reaction temperature between 60°C and 85°C. The benzoyl chloride was dropped in about 1.5 hours. After the dropwise addition, the reflux reaction was continued and samples were taken to track the reaction process. When the mass fraction of benzoyl chloride in the reaction solution was less than 0.1%, the reaction was over, and it took about 4 hours. After cooling down to 35°C-45°C, filter, wash the filter residue twice with 40mL tol...

Embodiment 4

[0023] The synthetic method of embodiment four benzoyl cyanides

[0024] Put 100mL of toluene, 23.7g of 97% solid sodium cyanide, 0.3g of polyethylene glycol 600, 0.3g of trioctylmethylammonium chloride, and 0.6g of water into a 250mL four-necked flask, turn on the tail gas absorption device, stir, Circulating cooling water. Turn on the heating device and start heating. When the temperature of the reaction solution rose to 85°C, the cock of the constant pressure dropping funnel was opened, and 57.4g of benzoyl chloride was added dropwise, taking care to maintain the reaction temperature between 85°C and 110°C. The benzoyl chloride was dropped in about 1.5 hours. After the dropwise addition, the reflux reaction was continued and samples were taken to track the reaction process. When the mass fraction of benzoyl chloride in the reaction solution was less than 0.1%, the reaction was over, and it took about 4 hours. After cooling down to 35°C-45°C, filter, wash the filter residu...

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Abstract

The invention discloses a synthesis method of benzoyl cyanide. The method is characterized in that sodium cyanide and benzoyl chloride are taken as raw materials, the mixture of polyethylene glycol 600 and trioctylmethylammonium chloride is taken as a phase transferring catalyst, water or glycerol is taken as an auxiliary catalyst, the reaction with the benzoyl chloride is conducted at the temperature of 60 DEG C-110 DEG C, a benzoyl cyanide coarse product and a reaction bi-product are prepared after the reaction is conducted for 3-5 hours, and the coarse product is washed and separated to prepare a benzoyl cyanide fine product under the action of a solvent. The method has the advantages that the benzoyl cyanide is synthesized through a simple method, an alkaline chlorination method is adopted to perform treatment in order to reduce pollution and turn harm into benefit, and therefore cyanide is oxidized and destructed by active chlorine under strong alkaline conditions to generate atoxic sodium chloride; the solvent can be recycled, so that the synthesis method has the advantages of low pollution, high conversion, simple operation and the like.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for synthesizing benzoyl cyanide. Background technique [0002] Benzoyl cyanide is a colorless squamous crystal at room temperature. It is an important fine chemical intermediate, which is widely used in the synthesis of pesticides and medicines, such as: the herbicide fenmetrione, benzazine, and the medicine Weichangning Wait. The synthesis methods of benzoyl cyanide include: reaction method of benzoyl chloride and cuprous cyanide, reaction method of benzoyl chloride and benzoic anhydride and sodium cyanide, dimethylamine catalyzed hydrocyanic acid method, sodium cyanide and benzoyl chloride Reaction method. However, the required reaction temperature of benzoyl chloride and cuprous cyanide reaction method is about 210°C higher, the required time is longer and the yield is low. Can reduce the consumption of cuprous cyanide, lower reaction temperature, but still can't sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/14C07C255/40
CPCC07C253/14C07C255/40
Inventor 徐国想徐松李绍锁汪港谷训刚李国庆张允冰刘学峰
Owner 江苏佳麦化工有限公司
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