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Preparation method of 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate

A technology of pyrazole sulfate and hydroxyethyl, which is applied in the field of preparation of 4,5-diamino-1-pyrazole sulfate, can solve the problems of complex synthesis process, long cycle and high synthesis cost, and achieve the benefit of The effect of expanding promotion, less by-products, and reducing synthesis cycle

Inactive Publication Date: 2019-11-08
YIXING XINYU CHEM
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Problems solved by technology

[0002] 4,5-diamino-1-(2-hydroxyethyl) pyrazole sulfate is as a kind of important intermediate, and prior art CN106279026A adopts 2-cyano-3-ethoxy ethyl acrylate as The starting material is cyclized with 2-hydroxyethylhydrazine in ethanol, and then obtained through hydrolysis, acidification, decarboxylation, nitrosation, reduction, and sulfuric acid salt formation. The synthesis method is complicated, the cycle is long, and the synthesis cost is low. very high

Method used

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Embodiment Construction

[0027] The concrete technical scheme of the present invention is described in conjunction with embodiment:

[0028] A kind of preparation method of 4,5-diamino-1-(2-hydroxyethyl) pyrazole sulfate, comprises the following steps:

[0029] (1) Add 100kg of water, 75kg of ethanol, and 100kg of 2-hydroxyethylhydrazine into the reactor in sequence. The pressure of the reactor is controlled at 0.3-0.4MPa, and the temperature is slowly heated to 72-74°C;

[0030] Mix 100kg of ethanol and 180kg of diethyl ethoxymethylenemalonate and heat to 45-50°C, stir until completely dissolved;

[0031] Drop the ethanol solution of diethyl ethoxymethylene malonate into the reaction kettle for 80-100 minutes, keep the temperature of the reaction kettle during the dropping process, and raise the temperature to 78-80°C after the dropping is completed , constant temperature for 3 to 5 hours to carry out the cyclization reaction;

[0032] (2) Dissolve 60kg of sodium hydroxide in 100kg of water to obta...

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Abstract

The invention relates to a preparation method of 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate. Diethyl ethoxymethylenemalonate is taken as an initial raw material and cyclized with 2-hydroxyethyl inethyl alcohol, and then the 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate is prepared through hydrolysis, acidization, decarboxylation, nitrosation, reduction and sulfuric acid salifying. Accordingto the preparation method of the 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate, by-products are few, a prepared product is high in purity, meanwhile a process is simplified, the synthesis period is shortened, and meanwhile expansion and popularization are also facilitated.

Description

technical field [0001] The present invention relates to a kind of preparation method of intermediate, more specifically, relate to a kind of preparation method of 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate. Background technique [0002] 4,5-diamino-1-(2-hydroxyethyl) pyrazole sulfate is as a kind of important intermediate, and prior art CN106279026A adopts 2-cyano-3-ethoxy ethyl acrylate as The starting material is cyclized with 2-hydroxyethylhydrazine in ethanol, and then obtained through hydrolysis, acidification, decarboxylation, nitrosation, reduction, and sulfuric acid salt formation. The synthesis method is complicated, the cycle is long, and the synthesis cost is low. very high. Contents of the invention [0003] The present invention aims at the above problems and provides a preparation method of 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate with simple process and high purity. [0004] In order to realize the above-mentioned purpose of the present invention...

Claims

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Application Information

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IPC IPC(8): C07D231/38
CPCC07D231/38
Inventor 袁顺福范洪振袁郡范琳许薇
Owner YIXING XINYU CHEM
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