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5-amino-1-methyl-1h-pyrazole-4-carboxylic acid ethyl ester synthesis process

A synthesis process and a pyrazolamine technology, applied in the field of pyrazolamine synthesis technology, can solve the problems of complex production process, low production efficiency, high cost and high cost, and achieve the effects of overcoming many processes, improving yield and improving work efficiency

Inactive Publication Date: 2016-06-08
吕艳
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

In the current synthesis process method of pyrazolamide, the technical process is not easy to implement, the resulting pyrazolamide product has low purity, the reaction residue cannot be recycled, the production process is complicated, the production efficiency is low and the cost is high, and it is not suitable for large-scale production. Production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0011] The pyrazolamide synthesis technique of the present embodiment comprises the following steps:

[0012] (1) Put ethyl ethoxymethylene cyanoacetate into the reaction kettle, inhale toluene, stir and dissolve, then inhale methylhydrazine into the dripping tank;

[0013] (2) Turn on the frozen brine, start adding methylhydrazine dropwise when it drops to 25°C, keep the temperature at 22°C, and keep warm for 3 hours after dropping;

[0014] (3) Then open the steam valve, slowly rise to the reflux temperature, reflux for 2 hours, turn on the refrigeration, cool down to 10°C and discharge, and dry the filter cake to obtain pyrazolamide.

[0015] The synthesis process of pyrazolamide does not require cumbersome post-reaction treatment, greatly improves product performance, is environmentally friendly and pollution-free, the process is easy to implement, low production cost, high synthesis yield, and better realizes the industrial production of products.

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Abstract

The present invention discloses a 5-amino-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester synthesis process, which is characterized in that a 40% methyl hydrazine aqueous solution and ethoxy methylene ethyl cyanoacetate are adopted as raw materials, and toluene is adopted as a solvent. According to the present invention, the raw material 40% methyl hydrazine solution has characteristics of easy obtaining, low damage on human body, high safety and low cost, the toluene is adopted as the solvent, and the synthesis process has characteristics of simple process, easy operation, substantially-shortened reaction time, high product yield, and no three-waste emission.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a pyrazolamide synthesis process. Background technique [0002] Pyrazolamide, also known as ethyl 5-amino-1-methylpyrazole-4-carboxylate, is mainly used as a pesticide intermediate and can be directly used to synthesize sulfonamides. In the current synthesis process method of pyrazolamide, the technical process is not easy to implement, the resulting pyrazolamide product has low purity, the reaction residue cannot be recycled, the production process is complicated, the production efficiency is low and the cost is high, and it is not suitable for large-scale production. Production. Contents of the invention [0003] In order to overcome the above-mentioned technical problems existing in the prior art, the object of the present invention is to provide a pyrazolamide synthesis process. The present invention not only has a simple production process and i...

Claims

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Application Information

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IPC IPC(8): C07D231/38
Inventor 吕艳
Owner 吕艳
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