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Industrial production method of 3, 5-Dimethylbenzoyl chloride

A technology of dimethylbenzoyl chloride and dimethylbenzoic acid, which is applied in the industrial production field of 3,5-dimethylbenzoyl chloride, can solve the problem of high usage of thionyl chloride, reduction of equipment production capacity, and recovery of energy. To solve the problem of high consumption, to achieve the effect of fast response, thorough response and low dosage

Inactive Publication Date: 2019-01-04
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of thionyl chloride in this process is extremely high, which is not suitable for industrial production, and the recovery energy consumption is high, and the production capacity of the equipment is also reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The industrial production method of described 3,5-dimethylbenzoyl chloride, the steps are as follows:

[0024] (1) Add 1500g of 3,5-dimethylbenzoic acid and 1785g of thionyl chloride into the reaction kettle, and control the reaction temperature at 40°C for 1.5 hours under ultrasonic conditions;

[0025] (2) be warming up to reflux, react 1.5 hours;

[0026] (3) Thionyl chloride was recovered by distillation, and then distilled at -0.098MPa to obtain a colorless liquid 3,5-dimethylbenzoyl chloride product with a yield of 99.25%.

Embodiment 2

[0028] The industrial production method of described 3,5-dimethylbenzoyl chloride, the steps are as follows:

[0029] (1) Add 1500g of 3,5-dimethylbenzoic acid and 1785g of thionyl chloride into the reaction kettle, and control the reaction temperature at 50°C for 0.5 hours under ultrasonic conditions;

[0030] (2) be warming up to reflux, react 2 hours;

[0031] (3) Thionyl chloride was recovered by distillation, and then distilled at -0.098MPa to obtain a colorless liquid 3,5-dimethylbenzoyl chloride product with a yield of 98.75%.

Embodiment 3

[0033] The industrial production method of described 3,5-dimethylbenzoyl chloride, the steps are as follows:

[0034] (1) Add 1500g of 3,5-dimethylbenzoic acid and 2380g of thionyl chloride into the reaction kettle, and control the reaction temperature at 30°C for 2 hours under ultrasonic conditions;

[0035] (2) be warming up to reflux, react 1 hour;

[0036] (3) Thionyl chloride was recovered by distillation, and then distilled at -0.098MPa to obtain a colorless liquid 3,5-dimethylbenzoyl chloride product with a yield of 99.12%.

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Abstract

The invention belongs to the technical field of fine chemical industry, which particularly relates to an industrial production method of 3, 5-Dimethylbenzoyl chloride. The production method of 3, 5-dimethylbenzoyl chloride comprises the following steps: (1) adding 3,5-Dimethylbenzoic acid and thionyl chloride into a reaction kettle, controlling the reaction temperature to be 30-50 DEG C for 0.5 to2 hours under the ultrasonic condition; (2) heating to reflux and reacting for 1 to 2 hours; (3) distilling and recovering thionyl chloride to obtain 3, 5-Dimethylbenzoyl chloride products. The thionyl chloride thereof is not only used as an acyl chloride reagent but also serves as a solvent. The reaction is carried out under the ultrasonic condition, having the advantages of high speed and smallreaction solvent in uses, low energy consumption for collection. The method is suitable for industrial production. The reflux reaction is carried out by adopting a heat preservation reaction. The reaction temperature of the thermal insulation reaction is low, and the reaction is mild without generating impurities. The reflux reaction is thorough, improving the purity of the product.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to an industrial production method of 3,5-dimethylbenzoyl chloride. Background technique [0002] 3,5-Dimethylbenzoyl chloride is an important chemical intermediate, mainly used in the production of medicines, pesticides, and intermediates in the production of dyes and photosensitive materials. It is used to synthesize mites (tebufenozide) in the production of pesticides. There is also methoxyfenozide, which has high economic value. [0003] In recent years, with the continuous expansion of the application range of 3,5-dimethylbenzoyl chloride, the research on its synthesis process by various scientific research institutions is also deepening. [0004] Shandong Pesticide Research Institute has a report "Methoxyfenozide" in "Modern Pesticides 2003", which introduces the reaction of 3,5-dimethylbenzoic acid and thionyl chloride under the condition of using toluene as solvent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/04C07C51/60
CPCC07C51/60C07C63/04
Inventor 肖志宇韩楠楠王荣海张瑞光黄玉亭韩谆谆
Owner SHANDONG KAISHENG NEW MATERIALS
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