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Preparation method of dimethylcarbamoyl chloride

A technology of dimethylcarbamoyl and dimethylamine, which is applied in the field of preparation of dimethylcarbamoyl chloride, can solve the problems of difficult separation of toluene and products, low yield, cumbersome operation, etc., and achieve good application value and application prospect , simple operation, high content effect

Inactive Publication Date: 2019-02-22
湖南海利常德农药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defects of this method are obvious: the yield is not high, the amount of three wastes is large, the separation of toluene and the product is difficult, and the operation is cumbersome

Method used

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  • Preparation method of dimethylcarbamoyl chloride
  • Preparation method of dimethylcarbamoyl chloride
  • Preparation method of dimethylcarbamoyl chloride

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Embodiment 1

[0024] The invention relates to a preparation method of dimethylcarbamoyl chloride. A microreactor is used as a reaction device, and dimethylamine and phosgene are simultaneously passed into the microreactor for reaction to obtain dimethylcarbamoyl chloride. Include the following steps:

[0025] A microreactor with 8 reaction templates was used as the reaction device, and the temperature of each reaction module in the microreactor was controlled at 190 °C. By gas mass flow meter, 136.4g dimethylamine (99.0%, 3.0mol) is passed in the microreactor with the speed of 68.2g / min, simultaneously with 371.3g phosgene (80%, 3.0mol) with the speed of 185.7g / min mol) into the microreactor, mixed and reacted; after the reaction was completed, the obtained gas material was cooled to room temperature and condensed with a cooling device, and the cooled liquid material was collected to obtain 325.4g dimethylcarbamoyl chloride crude product; After distillation, 310.1 g of dimethylcarbamoyl ch...

Embodiment 2

[0027] The invention relates to a preparation method of dimethylcarbamoyl chloride. A microreactor is used as a reaction device, and dimethylamine and phosgene are simultaneously passed into the microreactor for reaction to obtain dimethylcarbamoyl chloride. Include the following steps:

[0028] A microreactor with 8 reaction templates was used as the reaction device, and the temperature of each reaction module in the microreactor was controlled at 190 °C. Through the gas mass flow meter, 136.4g dimethylamine (99.0%, 3.0mol) is passed in the microreactor with the speed of 68.2g / min, simultaneously with the speed of 204.2g / min 408.4g phosgene (80%, 3.3 mol) into the microreactor, mixed and reacted; after the reaction was completed, the obtained gas material was cooled to room temperature with a cooling device, condensed, and the cooled liquid material was collected to obtain 324.1g dimethylcarbamoyl chloride crude product; After distillation, 311.8g of dimethylcarbamoyl chlori...

Embodiment 3

[0030] The invention relates to a preparation method of dimethylcarbamoyl chloride. A microreactor is used as a reaction device, and dimethylamine and phosgene are simultaneously passed into the microreactor for reaction to obtain dimethylcarbamoyl chloride. Include the following steps:

[0031] A microreactor with 8 reaction templates was used as the reaction device, and the temperature of each reaction module in the microreactor was controlled at 200 °C. By gas mass flow meter, 136.4g dimethylamine (99.0%, 3.0mol) is passed in the microreactor with the speed of 27.3g / min, simultaneously with 371.3g phosgene (80%, 3.0mol) with the speed of 74.3g / min mol) into the microreactor, mixed and reacted; after the reaction was completed, the obtained gas material was cooled to room temperature and condensed with a cooling device, and the cooled liquid material was collected to obtain 326.7g of dimethylcarbamoyl chloride crude product; After distillation, 313.4g of dimethylcarbamoyl c...

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Abstract

The invention discloses a preparation method of dimethylcarbamoyl chloride. The preparation method comprises the following steps: simultaneously introducing dimethylamine and phosgene into a micro-reactor to perform the reaction to obtain the dimethylcarbamoyl chloride. The dimethylcarbamoyl chloride prepared in the preparation method disclosed by the invention is high in content, the content reaches 98.5 to 99 percent, and the yield is greatly increased and can reach 95.0 to 96.2 percent (referring to dimethylamine). The preparation method disclosed by the invention has the advantages of simple operation, high yield, less waste, safety, environmental protection and the like, is suitable for industrialized production and good in application value and application prospect.

Description

technical field [0001] The invention relates to a preparation method of dimethylcarbamoyl chloride. Background technique [0002] Dimethylcarbamoyl chloride, English name: Dimethylcarbamoyl chloride, is an intermediate of carbamate insecticides such as pirimicarb, pyrimicarb, etc., and is also used as an intermediate for medicine, dyes, synthetic materials and other fine chemicals , such as for the production of neostigmine bromide, neostigmine methylsulfate, pyridostigmine, etc. The structural formula is as follows: [0003] [0004] At present, there are very few manufacturers of this product in China, and there are few related synthesis reports. [0005] In the article published in 1950, R.J.SLOCOMBE, EDGAR E.HARDY, J.H.SAUNDRRS.1ND R.L. reported the method of synthesizing dimethylcarbamoyl chloride in a self-made glass reaction vessel by the gas phase method at 275 ° C. The reported yield was 90%; the method has the disadvantages of high reaction temperature, low y...

Claims

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Application Information

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IPC IPC(8): C07C269/00C07C271/04
CPCC07C269/00C07C271/04
Inventor 王胜得曾敬陈明吴曼刘伟曾雪云徐建兵竺来发高云英
Owner 湖南海利常德农药化工有限公司
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