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Methyl carbamate refining method

A technology of methyl carbamate and refining method, which is applied in the field of methyl carbamate refining to achieve the effects of reasonable process, high purity and convenient operation

Pending Publication Date: 2022-06-24
山东禹城易澳科技有限公司
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for refining methyl carbamate to solve the problem that existing methyl carbamate products contain trace amounts of ethyl carbamate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0017] A method for purifying methyl carbamate, the concrete purifying method steps are as follows:

[0018] (1) Add 10 g of methyl carbamate and toluene (100 mL, 10 times the volume) to a round-bottomed flask at 30ºC (permissible range 25-35ºC) (Note: the material is hygroscopic and should be kept under nitrogen conditions) treatment); heat and raise the temperature of the reaction mass to 53°C (permissible range 50-56ºC) (note: a clear and homogeneous solution should be observed); slowly cool the reaction mass to 30°C (permissible range 25-35°C) °C) (note: product formation was observed at 35-40 °C); the reaction mass was stirred at 30 °C (the allowable range was 25-35 °C) for 15-30 min; the reaction mass was further cooled to 3 °C (allowable range was 25-35 °C) The range is 0-6°C); at 3°C ​​(the allowable range is 0-6°C), stir the reaction material for 1h (1h±15min); filter the reactant, suck dry until the filtrate is completely discharged;

[0019] (2) Wash the wet produc...

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Abstract

According to the methyl carbamate refining method, methyl carbamate is subjected to recrystallization separation and vacuum drying treatment through methylbenzene under nitrogen protection, ethyl carbamate is separated out, and a refined methyl carbamate product is obtained. The methyl carbamate is recrystallized and purified for multiple times by adopting methylbenzene, so that the ethyl carbamate in the methyl carbamate is separated out, the impurity of the ethyl carbamate is reduced to a level which cannot be detected, and the method has the advantages of reasonable process, convenience in operation and high purity.

Description

technical field [0001] The invention relates to the technical field of organic synthesis intermediate processing, in particular to a method for purifying methyl carbamate. Background technique [0002] Methyl carbamate is an important organic synthesis intermediate, which can be used as an organic synthesis intermediate in medicine, pesticide and other industries. It has the characteristics of low toxicity, strong poisoning specificity, easy to be degraded by various factors, low residue, and small side effects on the environment, so it has become a new type of insecticide, herbicide, and mosquito and fly control in the world in recent years. agent, and its application field is expanding rapidly. Methyl carbamate products in the existing process contain trace amounts of urethane. Ethyl carbamate is a carcinogen that can cause lung tumors, lymphoma, liver cancer, skin cancer, etc. How to remove carbamate from methyl carbamate products? The separation of ethyl ester impuriti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C269/08C07C271/12
CPCC07C269/08C07C271/12
Inventor 张振忠李龙动李龙存孙加强
Owner 山东禹城易澳科技有限公司
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