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Synthetic method of adipic dihydrazide

A technology of adipic acid dihydrazide and a synthetic method, which is applied in the field of chemical synthesis, can solve problems such as being unsuitable for industrialized production, producing many impurities in by-products, complicated synthesis process, etc., and achieve simple post-treatment process, high purity of the product, The effect of simple synthetic route

Active Publication Date: 2018-06-22
JIANGSU LINGYUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first step of the esterification reaction, most of them use concentrated sulfuric acid as a catalyst, which has problems such as strong corrosion, large amounts of organic waste water, serious environmental pollution, and many by-products and impurities. Environmentally friendly catalysts such as Although solid acids and heteropoly acids are getting more and more attention, they generally have problems such as relatively high production costs and cumbersome synthesis processes, which are more suitable for scientific research, and there are still many problems to be solved in actual production.
In addition, the above two synthetic methods all need expensive raw material hydrazine hydrate, the production cost is high, and it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 17.4g (0.1mol) dimethyl adipate into a four-necked flask with a stirring bar, a thermometer and a separatory funnel, then add 28g (0.25mol) acetonazine, heat to 50°C, and stir at a constant speed. Until the two are completely miscible, a mixed solution is obtained; continue to heat the mixed solution, and when the temperature of the mixed solution reaches 120°C, slowly add 9 g (0.5 mol) of water to the mixed solution from the separatory funnel, and the dropping speed is 25-30 second / drop, and at the same time, add 11g of catalyst D072 macroporous strongly acidic styrene-based cation exchange resin, and ensure that the system temperature is reacted at 120°C for about 3 hours until dimethyl adipate is completely reacted to obtain the reaction product diacyl adipate Hydrazine; distill all the unreacted acetonazine and water, crystallize the solid in the flask, wait until the temperature of the system drops to about 20°C, and then wash the above solid with absolute ethan...

Embodiment 2

[0023] Add 17.4g (0.1mol) dimethyl adipate into a four-necked flask with a stirring bar, a thermometer and a separatory funnel, then add 28g (0.25mol) acetonazine, heat to 40°C, and stir at a constant speed. Until the two are completely miscible, a mixed solution is obtained; continue to heat the mixed solution, and when the temperature of the mixed solution reaches 128° C., slowly add 9 g (0.5 mol) of water to the mixed solution from the separatory funnel, and the dropping speed is 25-30 second / drop, and at the same time, add 11g of catalyst 001×2 strong acidic styrene-based cation exchange resin to ensure that the system temperature is kept at 128°C for about 3 hours until the dimethyl adipate is completely reacted to obtain the reaction product adipyl diacyl Hydrazine; distill all the unreacted acetonazine and water, crystallize the solid in the flask, wait until the temperature of the system drops to about 25°C, then wash the above solid with propanol for 3-5 times, Put it...

Embodiment 3

[0025] Add 26.1g (0.15mol) of dimethyl adipate into a four-neck flask equipped with a stirring bar, a thermometer and a separatory funnel, then add 50.4g (0.45mol) of acetonazine, heat to 50°C, and stir at a constant speed , until the two are completely miscible to obtain a mixed solution; continue to heat the mixed solution, and when the temperature of the mixed solution reaches 120°C, slowly add 16.2g (0.9mol) of water from the separating funnel to the mixed solution at a dropping speed of 25 -30 seconds / drop, at the same time, add 18.5g of catalyst D072 macroporous strongly acidic styrene-based cation exchange resin, and ensure that the system temperature is reacted at 125°C for about 3 hours until the dimethyl adipate is completely reacted to obtain the reaction product adipic di Acid dihydrazide; distill all the unreacted acetonazine and water, crystallize the solid in the flask, and wait until the temperature of the system drops to about 25°C, then wash the above solid wi...

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PUM

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Abstract

The invention discloses a synthetic method of adipic dihydrazide. According to the method, dimethyl adipate, acetone azine and water are taken as raw materials, a catalyst is added to a system at certain temperature, after reaction is performed for a period of time, a reaction product is subjected to distillation, crystallization, washing and drying treatment, and obtained white solid is the target product adipic dihydrazide. The synthetic route is simple, and product yield is high; fewer byproducts and impurities are produced, postprocessing is simple, and product purity is high; three wastesare not produced in the synthetic process, the method is environmentally friendly and suitable for industrial production, and raw material cost is lower.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing adipic acid dihydrazide. Background technique [0002] Adipic acid dihydrazide (ADH), also known as Jidihydrazide, is a white crystalline powder and a bifunctional compound. It can be used for cross-linking in water-based resins; it can be used as a protein drug carrier after cross-linking with sodium hyaluronate, and can be used in the medical field; it can also be used as indoor formaldehyde adsorbent and intermediate raw materials. [0003] At present, the methods for synthesizing adipate dihydrazide in the prior art are mainly divided into two types, that is, one-step synthesis method and two-step synthesis method. The one-step synthesis method is to use adipic acid and hydrazine hydrate to directly react to generate adipate dihydrazide: adipic acid and hydrazine hydrate are refluxed for a certain period of time under heating conditions, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/04C07C243/28
CPCC07C241/04C07C243/28
Inventor 凌青云毕亚铃蒋忠良
Owner JIANGSU LINGYUN PHARMA
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