Preparation method of p-anisoyl chloride

A technology of methoxybenzoyl chloride and methoxybenzoic acid, which is applied in the field of preparation of p-methoxybenzoyl chloride, can solve the problems of environmental pollution, toxicity, and high requirements for use and transportation, and achieves reduction of environmental pollution, reduction of The effect of loss

Active Publication Date: 2012-08-08
江苏万隆化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The thionyl chloride used in the above preparation process of p-methoxybenzoyl chloride has serious corrosion on equipment, high requirements for use and transportation, and high price
In addition, the existing p-methoxybenzoyl chloride preparation process contains a large amount of toxic and difficult-to-handle sulfur dioxide in the tail gas generated during synthesis, which is easy to cause environmental pollution
In addition, highly toxic phosgene, phosphorus trichloride, phosphorus pentachloride, etc. are used as chlorinating agents. The use of the above substances and the discharge of waste will cause serious pollution to the environment.

Method used

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  • Preparation method of p-anisoyl chloride
  • Preparation method of p-anisoyl chloride
  • Preparation method of p-anisoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The p-methoxybenzoyl chloride preparation method of the present embodiment is as figure 1 As shown, the specific process is:

[0021] 1) Add 1 mol trichlorotoluene and 0.5 g of zinc chloride to the reaction bottle, open the stirrer inserted into the reaction bottle, add 1 mol p-methoxybenzoic acid, heat up to 150 ° C in 1 hour, keep the temperature for 5 hours, and react The tail gas in the water is absorbed into 30% hydrochloric acid;

[0022] 2) After the reaction, cool the temperature of the reaction material in the reaction bottle to 25°C, add 1g of hydroquinone, transfer the reaction material in the reaction bottle to the rectification column for vacuum distillation (the rectification column adopts Φ24* 1500, glass filler); finally obtain p-methoxybenzoyl chloride 165g, obtain benzoyl chloride 133g simultaneously.

[0023] The content of p-methoxybenzoyl chloride is 99.5%, the content of benzoyl chloride is 99.7%, the yield of benzoyl chloride is 95%, and the yie...

Embodiment 2

[0025] The p-methoxybenzoyl chloride preparation method of the present embodiment is basically the same as embodiment one, and the difference is: 1. in the 1) step, replace zinc chloride 0.5g with ferric chloride 0.5g; 2. through 1 3. react for 6 hours; 4. in 2) step, the cooling temperature of material is 15 ℃; 5. finally obtain p-methoxybenzoyl chloride 163g, obtain benzoyl chloride 131g simultaneously.

[0026] The content of benzoyl chloride was 99.7%, the content of p-methoxybenzoyl chloride was 99.5%, the yield of benzoyl chloride was 95%, and the yield of p-methoxybenzoyl chloride was 97% by gas chromatography AG6820.

Embodiment 3

[0028] The concrete process of the p-methoxybenzoyl chloride preparation method of the present embodiment is:

[0029] 1) Add 600kg of trichlorotoluene and 456kg of p-methoxybenzoic acid into the glass-lined reactor, add 0.5kg of Lewis acid catalyst at the same time, stir, first raise the temperature to 80 degrees for 1 hour, then raise the temperature to 130 degrees for 1 hour , and finally raised the temperature to 150°C, and reacted at a constant temperature for 10 hours, and the tail gas in the reaction was absorbed by water to become 30% hydrochloric acid;

[0030] 2) the temperature of the reaction material in the reactor is cooled to 20°C, and is transferred to a 15-meter high rectification tower (the rectification tower adopts an enamel corrugated packing tower), and 0.5kg of hydroquinone is added, and rectification under reduced pressure is carried out to obtain the Methoxybenzoyl chloride 496kg and benzoyl chloride 409kg.

[0031] The content of benzoyl chloride was...

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Abstract

The invention relates to a preparation method of p-anisoyl chloride and belongs to the technical field of carbocyclic compounds. The preparation method comprises the following steps that raw materials of benzotrichloride and p-methoxybenzoic acid are mixed by stirring according to a mole ratio of 1: 1; the mixture undergoes an acyl chlonnation reaction in the presence of a lewis acid catalyst at a temperature of 100 to 150 DEG C for 5 to 10 hours; acyl chlonnation reaction products are cooled to a temperature of 20+ / -5 DEG C; the cooled acyl chlonnation reaction products are added with hydroquinone and then are purified so that p-anisoyl chloride and a by-product are obtained. Through the preparation method, low-cost, low-pollution and high-yield p-anisoyl chloride can be synthesized directly and simultaneously, the by-product of benzoyl chloride is obtained. In addition, the preparation method has the advantages that 1, tail gas produced by the preparation method can be absorbed by water and then is prepared into hydrochloric acid for recycle so that environmental pollution is reduced; and 2, the raw materials adopted by the preparation method do not corrode equipment so that an equipment loss is reduced.

Description

technical field [0001] The invention relates to a preparation method of p-methoxybenzoyl chloride, which belongs to the technical field of carbocyclic compounds. Background technique [0002] p-Methoxybenzoyl chloride is an intermediate used in the preparation of drugs such as piracetam, amiodarone, encaine hydrochloride, anistan, scutellarin and benzbromarone. [0003] The currently known process for preparing p-methoxybenzoyl chloride is: to react p-methoxybenzoic acid and thionyl chloride under reflux for 6 hours, recover thionyl chloride, and obtain pure p-methoxybenzoyl chloride by distillation under reduced pressure. Benzoyl chloride produces a large amount of by-product hydrogen chloride and sulfur dioxide in the reaction process simultaneously, and the reaction process of this method is shown in the following formula: [0004] [0005] The thionyl chloride used in the above preparation process of p-methoxybenzoyl chloride has serious corrosion to equipment, high ...

Claims

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Application Information

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IPC IPC(8): C07C65/21C07C63/10C07C51/60
Inventor 吴勇才史丽娟
Owner 江苏万隆化学有限公司
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