A kind of preparation method of 1,2-dimethyl-3-phenylpyrazoline perchlorate

A technology of dimethyl hydrazine and agitator, applied in the field of high-purity preparation, can solve problems such as waste of resources and environmental pollution, and achieve the effects of cost reduction, simple and easy operation of equipment, and realization of commercial large-scale production.

Active Publication Date: 2022-05-13
DONGLI NANTONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention solves the problem that the by-product 1,2-dimethylhydrazine in the industrial waste discharged during the synthesis of monomethylhydrazine can be fully utilized, and avoids environmental pollution and waste of resources caused by such dangerous compounds. Waste liquid can better realize the problem of turning waste into treasure, and invented a method of using industrial waste containing by-product 1,2-dimethylhydrazine in the production process of monomethylhydrazine to realize it through the conventional mannich reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 1,2-dimethylhydrazine 60g (1mol), 120g acetophenone (1mol), 30g formaldehyde (1mol) and 300ml Mix with absolute ethanol, then heat the reaction mixture at the same temperature until 1,2-dimethyl-5-phenylpyrazoline is formed, acidify by adding appropriate 70% perchloric acid dropwise, cool and filter to obtain a brown solid, wash, The crude product was recrystallized with ethanol, suction filtered, and vacuum-dried at 60°C to obtain a yellow powder, 222g, with a yield of 81.1% and a purity of 95.4%.

Embodiment 2

[0015] In a three-necked round-bottomed flask equipped with a mechanical stirrer, dropping funnel and reflux condenser, take 60 g (1 mol) of 1,2-dimethylhydrazine, add a small amount of benzaldehyde-acetone mixture, stir and warm for 20 minutes, add 120 g of benzene Ethanone (1mol), 30g formaldehyde (1mol), a small amount of citric acid and 300ml isopropanol are mixed, then the reaction mixture is heated at the same temperature until 1,2-dimethyl-3-phenylpyrazoline is formed, dropwise Add appropriate 70% perchloric acid to acidify, cool and filter to obtain a white solid, wash, recrystallize the crude product with isopropanol, suction filter, and vacuum dry at 60°C to obtain a white crystalline powder. The product is 258g, with a yield of 94.3% and a purity of 99.4%. .

Embodiment 3

[0017] In a three-neck round-bottomed flask with a mechanical stirrer, dropping funnel and reflux condenser, take 60g (1mol) of 1,2-dimethylhydrazine, add a small amount of acetic anhydride acetone solution, stir and warm for 20min, add 120g of phenylethyl alcohol Ketone (1mol), 30g formaldehyde (1mol), a small amount of tert-butyl hydrodiphenol and citric acid, add 300ml isopropanol and mix, then heat the reaction mixture at the same temperature until 1,2-dimethyl-5-benzene Add appropriate 70% perchloric acid dropwise to acidify and cool and filter to obtain a white solid, wash, recrystallize the crude product with isopropanol, filter with suction, and dry under vacuum at 60°C to obtain a white crystalline powder. 256g of the product is obtained. Yield 93.7%, purity 99.5%.

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Abstract

A method of using industrial waste 1,2-dimethylhydrazine as a raw material to prepare high-purity 1,2-dimethyl-3-phenylpyrazoline chlorate, which is an important intermediate for medicine and pesticides body. In order to complete and overcome the shortcomings of hydrazine compound instability and reaction by-products, the present invention appropriately adds a related impurity protective agent and antioxidant in the starting material before the reaction, and carries out the mannich reaction in a higher alcohol solvent to obtain High-purity 1,2-dimethyl-3-phenylpyrazoline chlorate powder crystals, avoiding the complicated purification steps in industrial production with many residual types of final target impurities, and solving the problem of industrial production of high-purity 1, The conventional method of 2-dimethyl-3-phenylpyrazoline chlorate controls and eliminates all sources of impurities, and realizes the advantages of commercial scale production, cost reduction, and simple equipment.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a technical method for preparing high-purity 1,2-dimethyl-3-phenylpyrazoline chlorate by utilizing an industrial waste 1,2-dimethylhydrazine. Background technique [0002] my country is a big producer of monomethylhydrazine, and its annual output ranks among the top in the world. Monomethylhydrazine is a very valuable compound that is widely used in various industries such as medicine, pesticide, chemical industry, aerospace and missiles, and the production of this raw material is also increasing in large quantities with the large demand of the market. [0003] During the industrial preparation of monomethylhydrazine, by-products include 1,1-dimethylhydrazine and 1,2-dimethylhydrazine. The by-product of 1,1-dimethylhydrazine is separated and sold, which is an important raw material for the synthesis of rocket fuel and pharmaceutical intermediates. There is currently no known co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12
CPCC07D231/12
Inventor 阿依别克·马力克衣伟男周建
Owner DONGLI NANTONG CHEM
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