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Synthesis process of methyl cyanocarbamate

A technology for the synthesis of methyl cyanamide, which is applied in the field of synthesis of methyl cyanamide, can solve problems such as environmental pollution, difficult production of carbendazim, and high toxicity, and achieve the effect of reducing environmental pollution

Inactive Publication Date: 2020-10-30
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 synthetic technique of methyl cyanamide formate, synthetic technique comprises the following steps:

[0023] 1). Sodium metal is dissolved in propanol to form a sodium propoxide solution with a suitable concentration of propanol, which is blown into nitrogen for 30 minutes, and stored in cold storage for later use;

[0024] The mixing molar ratio of sodium propoxide and propanol is 1:100;

[0025] 2). Add lime nitrogen to cold water at 20°C for hydrolysis. After the hydrolysis is sufficient, filter it. The filtrate is heated to 90°C and then filtered while it is hot. At this time, the filtrate is kept at a constant temperature;

[0026] The mixing molar ratio of lime nitrogen and cold water is 1:20; the mixing molar ratio of lime nitrogen and propanol is 3:10;

[0027] 3). Add the pH regulator dilute hydrochloric acid dropwise to the filtrate in step 2, mix the solution evenly at a stirring rate of 1000r / min while adding, adjust the pH to 4, and then store at...

Embodiment 2

[0035] A kind of synthetic technique of methyl cyanamide formate, synthetic technique comprises the following steps:

[0036] 1). Sodium metal was dissolved in propanol to form a sodium propoxide solution with proper concentration of propanol, and nitrogen was blown in for 10 minutes, and it was stored in cold storage for later use;

[0037] The mixing molar ratio of sodium propoxide and propanol is 1:70;

[0038] 2). Add lime nitrogen to cold water at 10°C for hydrolysis. After the hydrolysis is sufficient, filter it. The filtrate is heated to 80°C and then filtered while it is hot. At this time, the filtrate is kept at a constant temperature;

[0039] The mixing molar ratio of lime nitrogen and cold water is 1:10; the mixing molar ratio of lime nitrogen and propanol is 1:3;

[0040] 3). Add the pH regulator dilute sulfuric acid dropwise to the filtrate in step 2, mix the solution evenly at a stirring rate of 500 r / min while adding, adjust the pH to 1, and then store at a co...

Embodiment 3

[0048] A kind of synthetic technique of methyl cyanamide formate, synthetic technique comprises the following steps:

[0049] 1). Sodium metal is dissolved in propanol to form a sodium propoxide solution with a suitable concentration of propanol, which is blown into nitrogen for 20 minutes, and stored in cold storage for later use;

[0050] The mixing molar ratio of sodium propoxide and propanol is 1:80;

[0051] 2). Add lime nitrogen to cold water at 15°C for hydrolysis, and then filter it after the hydrolysis is sufficient. The filtrate is heated to 85°C and then filtered while it is hot. At this time, the filtrate is kept at a constant temperature;

[0052]The mixing molar ratio of lime nitrogen and cold water is 1:15; the mixing molar ratio of lime nitrogen and propanol is 1:3;

[0053] 3). Add dropwise a mixture of pH regulator dilute hydrochloric acid, dilute sulfuric acid and dilute nitric acid to the filtrate in step 2, mix the solution evenly at a stirring rate of 80...

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PUM

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Abstract

The invention relates to a synthesis process of methyl cyanocarbamate. The synthesis process comprises the following steps: adding sodium metal to prepare a sodium propoxide solution of propyl alcohol, hydrolyzing lime nitrogen, carrying out filtering, adding acid into a filtrate to adjust a pH value, and transferring the filtrate into an esterification kettle; adding the sodium propoxide solutionand methyl propyl carbonate and carrying out a reaction; adding water into reaction liquid for extraction, and separating out an organic phase; rectifying the organic phase to obtain a solvent, and finally, conducting treatment with an electrodialyzer to obtain high-purity cyanamide methyl formate. According to the synthesis process of methyl cyanocarbamate, carbonic ester is used for replacing common methyl chloroformate, so introduction of high-harm liquid chlorine and phosgene is avoided, and environmental pollution is reduced; moreover, sodium propoxide is used as a catalyst for catalysisso as to realize smooth reaction, propyl alcohol generated in the reaction can be distilled out in time, and the catalyst can be recycled in time; lime nitrogen is filtered firstly after being hydrolyzed, so high-toxicity by-products generated in a later reaction are avoided; and the purity of the finally obtained methyl cyanocarbamate can reach 90% or above, and the yield of methyl cyanocarbamate can reach 85% or above.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, more specifically to a synthesis 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 synthesis, bu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/00C07C269/08C07C271/10
CPCC07C269/00C07C269/08C07C2531/02C07C271/10Y02P20/584
Inventor 过学军袁树林金斐丁锐马军
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD