Method for synthesizing acetamidine, acetamidine, application of acetamidine, and vitamin B1

A technology of acetamidine and acetamidine hydrochloride, which is applied in the field of compound synthesis, can solve problems affecting the reaction yield of acetamidine, and achieve the effects of reducing production costs, reducing moisture content, and increasing yield

Active Publication Date: 2020-04-17
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, when utilizing acetamidine hydrochloride and sodium methylate to react to synthesize acetamidine, after filtering the product obtained by the reaction, the obtained mother liquor is concentrated, and the water content in the concentrated mother liquor is 1% to 2%, and the water content is relatively high; in addition, Water will destroy the reaction product acetamidine in the reaction system, and the specific reaction equation is as follows: Therefore, the reaction yield of acetamidine will be affected in the presence of water

Method used

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  • Method for synthesizing acetamidine, acetamidine, application of acetamidine, and vitamin B1
  • Method for synthesizing acetamidine, acetamidine, application of acetamidine, and vitamin B1
  • Method for synthesizing acetamidine, acetamidine, application of acetamidine, and vitamin B1

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The method for synthesizing acetamidine comprises the following steps:

[0056]a, add the sodium methylate of 0.1 mol ratio (the mol ratio of sodium methylate and acetamidine hydrochloride) in acetamidine hydrochloride solid, make acetamidine hydrochloride and sodium methylate react, reaction temperature 20 ℃;

[0057] B, add 0.1 mol ratio (the mol ratio of methyl formate and acetamidine hydrochloride) to the reaction system in the reaction system Sodium methoxide, continue to keep warm for 1 hour;

[0058] c. After filtering the product obtained by the reaction in step b, collect the mother liquor, wash the filter cake sodium chloride with methanol, mix the washing liquid with the mother liquor, and concentrate (the conditions for concentration are: vacuum degree above -0.095Mpa, temperature 50°C, concentrate to constant weight), acetamidine was obtained.

Embodiment 2

[0060] The method for synthesizing acetamidine comprises the following steps:

[0061] a, add the sodium methylate of 0.3 mol ratio (the mol ratio of sodium methylate to acetamidine hydrochloride) in acetamidine hydrochloride solid, make acetamidine hydrochloride and sodium methylate react, reaction temperature 40 ℃;

[0062] B, add 0.2 mol ratio (the mol ratio of methyl formate and acetamidine hydrochloride) dewatering agent methyl formate in the reaction system, then add 1.7 mol ratio (the mol ratio of sodium methylate and acetamidine hydrochloride) in the reaction system Sodium methoxide, continue insulation reaction for 2 hours;

[0063] c. After filtering the product obtained by the reaction in step b, collect the mother liquor, wash the filter cake sodium chloride with methanol, mix the washing liquid with the mother liquor, and concentrate (the conditions for concentration are: vacuum degree above -0.095Mpa, temperature 50°C, concentrate to constant weight), acetamidin...

Embodiment 3

[0065] The method for synthesizing acetamidine comprises the following steps:

[0066] a, add the sodium methylate of 0.2 mol ratio (the mol ratio of sodium methylate to acetamidine hydrochloride) in acetamidine hydrochloride solid, make acetamidine hydrochloride and sodium methylate react, reaction temperature 30 ℃;

[0067] B, add 0.15 mol ratio (the mol ratio of methyl formate and acetamidine hydrochloride) dewatering agent methyl formate in the reaction system, then add 1.3 mol ratio (the mol ratio of sodium methylate and acetamidine hydrochloride) in the reaction system Sodium methoxide, continue the insulation reaction for 1.5 hours;

[0068] c. After filtering the product obtained by the reaction in step b, collect the mother liquor, wash the filter cake sodium chloride with methanol, mix the washing liquid with the mother liquor, and concentrate (the conditions for concentration are: vacuum degree above -0.095Mpa, temperature 50°C, concentrate to constant weight), ace...

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Abstract

The invention provides a method for synthesizing acetamidine, acetamidine and application thereof, and vitamin B1, belonging to the technical field of compound synthesis. The method for synthesizing the acetamidine comprises the following steps: reacting acetamidine hydrochloride with sodium methoxide to synthesize acetamidine, and adding methyl formate into a reaction system in the reaction process. The method is simple and convenient to operate, easy to implement and capable of effectively removing moisture in the acetamidine synthesis process and increasing the yield of acetamidine.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a method for synthesizing acetamidine, acetamidine and its application and vitamin B1. Background technique [0002] At present, when using acetamidine hydrochloride and sodium methylate to react to synthesize acetamidine, after filtering the product obtained by the reaction, the obtained mother liquor is concentrated, and the water content in the concentrated mother liquor is 1% to 2%, and the water content is relatively high; in addition, Water will destroy the reaction product acetamidine in the reaction system, and the specific reaction equation is as follows: Therefore, the reaction yield of acetamidine will be affected in the presence of water. [0003] In view of this, the present invention is proposed. Contents of the invention [0004] The object of the present invention is to provide a method for synthesizing acetamidine, which is simple, convenient and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/14C07D415/00
CPCC07C257/14C07D415/00
Inventor 李褦成陈英明郭军军许凡
Owner 江苏兄弟维生素有限公司
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