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Production process of methyl cyanocarbamate

A technology of methyl cyanamide formate and production process, applied in the field of drug synthesis, can solve the problems of difficult production of carbendazim, human injury, high toxicity, etc., achieve easy separation, recovery and recycling, reduce the release of pollutants, Speed ​​up the generated effect

Inactive Publication Date: 2020-09-29
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The consumption of methyl chloroformate in this method is relatively high, and the raw material liquid chlorine and methanol required for the synthesis of methyl chloroformate are relatively tight, which brings certain difficulties to the production of carbendazim.
[0003] Moreover, methyl cyanamide is colorless or has a little light blue aqueous solution, which is weakly alkaline and has a bad smell. It is also an important intermediate for the synthesis of carbendazim. In the process, phosgene and methanol and other related chemical substances are often used for synthesis, but phosgene is highly toxic, which will pollute the environment and cause harm to the human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of production technique of methyl cyanamide formate, production technique comprises the following steps:

[0023] 1). Sodium metal is dissolved in methanol to form a sodium methoxide solution with a suitable concentration of methanol. The mixing mass ratio of sodium methoxide to methanol is 1:150. Nitrogen gas is injected for 30 minutes, and it is refrigerated for later use;

[0024] 2). Add lime nitrogen to cold water at 20°C for hydrolysis. The mixing mass ratio of lime nitrogen and cold water is 1:150, and the mixing molar ratio of lime nitrogen and methanol is 3:7. After the hydrolysis is sufficient, filter it. After the filtrate is warmed up to 90°C, it is filtered while it is hot, and the filtrate is kept at a constant temperature at this time;

[0025] 3). First transfer the sodium methoxide solution of methanol into the esterification kettle, raise the temperature to 90°C, add dimethyl carbonate into the esterification kettle, and the mixing molar ratio o...

Embodiment 2

[0032] A kind of production technique of methyl cyanamide formate, production technique comprises the following steps:

[0033] 1). Sodium metal is dissolved in methanol to prepare a sodium methoxide solution with a suitable concentration of methanol. The mixing mass ratio of sodium methoxide and methanol is 1:100, and the mixing molar ratio of lime nitrogen and methanol is 2:5. Air for 10 minutes, refrigerated for later use;

[0034] 2). Add lime nitrogen to cold water at 20°C for hydrolysis. The mixing mass ratio of lime nitrogen and cold water is 1:100, and the mixing molar ratio of dimethyl carbonate and lime nitrogen is 1:1. After filtering, the filtrate is heated to 80°C and then filtered while it is hot, and the filtrate is kept at a constant temperature at this time;

[0035] 3). First transfer the sodium methoxide solution of methanol into the esterification kettle, raise the temperature to 80°C, add dimethyl carbonate into the esterification kettle, and mix the solu...

Embodiment 3

[0042] A kind of production technique of methyl cyanamide formate, production technique comprises the following steps:

[0043] 1). Sodium metal is dissolved in methanol to form a sodium methoxide solution with a suitable concentration of methanol. The mixing mass ratio of sodium methoxide to methanol is 1:120. Nitrogen gas is injected for 20 minutes, and it is refrigerated for later use;

[0044] 2). Add lime nitrogen to cold water at 15°C for hydrolysis. The mixing mass ratio of lime nitrogen and cold water is 1:100, and the mixing molar ratio of lime nitrogen and methanol is 1:2. After the hydrolysis is sufficient, filter it. After the filtrate is warmed up to 85°C, it is filtered while it is hot, and the filtrate is kept at a constant temperature at this time;

[0045] 3). First transfer the sodium methoxide solution of methanol into the esterification kettle, raise the temperature to 85°C, add dimethyl carbonate into the esterification kettle, and the mixing molar ratio o...

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Abstract

The invention relates to a production process of methyl cyanocarbamate. The method comprises the following steps: dissolving metallic sodium in methanol to prepare a sodium methoxide solution of methanol; hydrolyzing and filtering lime nitrogen, transferring a sodium methoxide solution of methanol into an esterification kettle, adding dimethyl carbonate into the esterification kettle, adding limenitrogen filtrate, hydrolyzing, esterifying, adding acid to adjust the pH value, adding water to extract and separate an organic phase, rectifying the organic phase, and reducing the ion concentrationby electrodialysis to obtain high-purity methyl cyanocarbamate. According to the production process of the methyl cyanocarbamate, the dimethyl carbonate is used for replacing methyl chloroformate, the consumption of liquid chlorine is reduced, and the release of pollutants in the production process of methyl chloroformate is also reduced; lewis base sodium methoxide is introduced in the preparation process to serve as a catalyst, so generation of methyl cyanocarbamate can be accelerated, the catalyst is easy to separate, recycle and reuse, the purity of the finally obtained methyl cyanocarbamate reaches 95% or above, and the yield reaches 90% or above.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, and more specifically relates to a production process of methyl cyanamide formate. Background technique [0002] Methyl cyanamide is an intermediate in the production of the fungicide carbendazim. The current post-filtration process is obtained by hydrolysis of lime nitrogen, amination of methyl chloroformate, and filtration. The consumption of methyl chloroformate in this method is relatively high, and the raw material liquid chlorine and methanol required for the synthesis of methyl chloroformate are relatively tight, which brings certain difficulties to the production of carbendazim. [0003] Moreover, methyl cyanamide is colorless or has a little light blue aqueous solution, which is weakly alkaline and has a bad smell. It is also an important intermediate for the synthesis of carbendazim. In the process, phosgene and methanol and other related chemical substances are often used for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/00C07C271/06C07C269/08B01J31/02
CPCB01J31/0212B01J2231/4283C07C269/00C07C269/08C07C271/06
Inventor 过学军袁树林金斐丁锐马军
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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