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Preparation method and device of hydroxyl pyrazol compound

A technology of hydroxypyrazoles and preparation device, applied in the direction of organic chemistry and the like, can solve the problems of inability to take into account economy, high efficiency, safety, etc., and achieve the effects of low cost, improved reaction efficiency, and improved heat dissipation problems

Inactive Publication Date: 2019-02-12
ASYMCHEM LAB FUXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The main purpose of the present invention is to provide a preparation method and device for hydroxypyrazole compounds, so as to solve the problem that economy, high efficiency and safety cannot be taken into account when synthesizing hydroxypyrazole compounds in the prior art

Method used

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  • Preparation method and device of hydroxyl pyrazol compound
  • Preparation method and device of hydroxyl pyrazol compound
  • Preparation method and device of hydroxyl pyrazol compound

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preparation example Construction

[0039] The above-mentioned preparation method comprises the following steps: alkoxy acrylate is used as raw material A, and As raw material B, raw material A and raw material B are continuously fed into the continuous reaction device for continuous reaction, and the crude product obtained by the reaction is continuously discharged from the continuous reaction device; wherein, formula I, formula II and wherein, R is H, an alkyl group, an unsaturated aliphatic hydrocarbon group, an aromatic group, an alkyl group containing a heteroatom, an unsaturated aliphatic hydrocarbon group containing a heteroatom or an aromatic group containing a heteroatom, and a hydroxypyrazole compound is obtained.

[0040] In the above-mentioned preparation method, adopt alkoxy acrylate and The reaction prepares the hydroxypyrazole compound, the route is shorter, the reaction efficiency is higher, and the cost is lower. At the same time, the present invention adopts a continuous reaction method to ...

Embodiment 1

[0060]

[0061] Heat the dry and clean continuous coil reactor to 120°C, take 1687.0g (16.0mol) of A, and put it in the feeding bottle 1. Get 1000.0g (16.0mol) 80% hydrazine hydrate and place it in the feeding bottle 2, and start feeding after the temperature of the coil pipe is stabilized, the feeding speed setting of the pump 1 (alkoxy acrylate): 31.4g / min, the 2 (hydrazine hydrate) feed rate setting: 18.6 g / min. The retention time of the reaction section is 30min, and the internal pressure is controlled at 1.0-2.0MPa. The discharge port is directly connected to the continuous crystallization-filtration system, and the crystallization is cooled at 10-20°C for a retention time of 30 minutes. Afterwards, the crystallization system passes through the continuous filtration system for solid-liquid separation. The separated filter cake was collected and dried at 40-50° C. to constant weight to obtain 1100.1 g of product with a purity of 99% and a yield of 90.2%.

Embodiment 2

[0063]

[0064] Heat the dry and clean continuous coil reactor to 120°C, take 1687.0g (16.0mol) of A, and put it in the feeding bottle 1. Take 2556.0g (16.0mol) of 40% methylhydrazine solution and put it in the feeding bottle 2, and start feeding after the coil temperature is stable, and the feeding speed setting of the pump 1 (alkoxy acrylate): 11.9g / min , pump 2 (40% methylhydrazine): 18.1 g / min. The retention time of the reaction section is 30min, and the internal pressure is controlled at 1.0-2.0MPa. The discharge port is directly connected to the continuous crystallization-filtration system, and the crystallization is cooled at 10-20°C for a retention time of 30 minutes. Afterwards, the crystallization system passes through the continuous filtration system for solid-liquid separation. The separated filter cake was collected and dried at 40-50° C. to constant weight to obtain 1297.1 g of product with a purity of 99% and a yield of 91.2%.

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Abstract

The invention provides a preparation method and device of a hydroxyl pyrazol compound. The preparation method comprises the steps that alkoxy acrylate serving as a raw material A and a raw material B(the formula is shown in the description) are continuously introduced into a continuous reaction device to be subjected to a continuous reaction, and a crude product obtained through the reaction is continuously discharged from the continuous reaction device, wherein R is H, alkyl, unsaturated aliphatic radical, aryl, alkyl containing heteroatoms, unsaturated aliphatic radical containing heteroatoms or aryl containing heteroatoms; the crude product is separated and purified to obtain the hydroxyl pyrazol compound. The alkoxy acrylate and the raw material B are adopted to react to prepare the hydroxyl pyrazol compound, the route is short, the reaction efficiency is high, and the cost is low. Meanwhile, the method adopts a continuous reaction means to synthesize the hydroxyl pyrazol compound, can effectively improve the heat dissipation problem in batch reaction process, and continuous reaction is beneficial for further improving the reaction efficiency.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method and device for hydroxypyrazole compounds. Background technique [0002] Hydroxypyrazoles, especially 1-substituted 5- or 3-hydroxypyrazoles are widely used in the preparation of medicines or plant herbicides. So far, the methods for preparing 1-substituted 5- or 3-hydroxypyrazoles usually include the following: [0003] Method 1: Hydrolysis of 2-methyl-1-(p-toluenesulfonyl)-3-pyrazolidinone or 2-methyl-1-1-acetyl-pyrazolidinone [sic] (J.Prakt. Chem. 313 (1971), 115-128 and J. Prakt. Chem. 313 (1971), 1118-1124). This method involves many steps and is complex. And the introduction and removal of protecting groups is difficult, meaning many extra steps are required and the yield is reduced. [0004] Method two: Alkyl 5-hydroxy-1-alkylpyrazole-4-carboxylate is synthesized by cyclization of dialkyl alkoxymethylene maleate and alkylhydrazine, and then to this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/20C07D231/22
CPCC07D231/20C07D231/22
Inventor 洪浩卢江平张恩选申慰闫红磊李广泽
Owner ASYMCHEM LAB FUXIN
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