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A kind of preparation technology of piperazine citrate

A technology for preparation of piperazine citrate, which is applied in the direction of organic chemistry, can solve the problems of unclear mechanism of action, large amount of waste liquid, cumbersome process, etc., and achieve low equipment requirements, simple operation, and simple process Effect

Active Publication Date: 2016-03-16
KAMP PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, this product can also be used to drive out pinworms, but its mechanism of action is not yet clear
[0003] The traditional preparation process of piperazine citrate is to use citric acid and piperazine hexahydrate as raw materials, and use water as solvent to prepare through dissolution, salt formation, alcohol precipitation, centrifugation, and drying. The process is cumbersome and produces a large amount of waste liquid Large, low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 4000 ml of 384.2 g of citric acid in ethanol to a 10000 ml reaction kettle and heat to 45°C; add dropwise 3000 ml of 258.5 g of anhydrous piperazine in ethanol to the reaction kettle. The dropwise addition time was 30 minutes. After the dropwise addition was completed, the reaction was carried out with heat preservation and stirring for 2 hours, then the stirring was stopped, cooling and crystallization, and centrifugal drying. 582 g of piperazine citrate was obtained, with a content of 99.2%, and a yield of 90.6%.

Embodiment 2

[0024] Add 4500 ml of 384.2 g of citric acid in ethanol to a 10000 ml reaction kettle, and heat to 60° C.; add dropwise 3000 ml of 258.5 g of anhydrous piperazine in ethanol to the reaction kettle. The dropwise addition time was 40 minutes. After the dropwise addition was completed, the reaction was carried out with heat preservation and stirring for 3 hours, then the stirring was stopped, cooling and crystallization, and centrifugal drying. 595g of piperazine citrate was obtained with a content of 99.7% and a yield of 92.6%.

Embodiment 3

[0026] Add 5000ml of 384.2g citric acid solution in acetone to a 10000ml reactor, and heat to 50°C; add dropwise 2500ml of anhydrous piperazine solution in 258.5g into the reactor. The dropwise addition time was 30 minutes. After the dropwise addition was completed, the reaction was carried out with heat preservation and stirring for 3 hours, then the stirring was stopped, cooling and crystallization, and centrifugal drying. 588g of piperazine citrate was obtained with a content of 99.4% and a yield of 91.5%.

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Abstract

The present invention relates to a piperazine citrate preparation method, and further provides a piperazine citrate with characteristics of safe quality and good stability. The preparation method comprises that: citric acid and anhydrous piperazine are completely dissolved and filtered, and form a salt in a reaction kettle under an appropriate reaction condition, and cooling crystallization, centrifugation, washing and vacuum drying are performed after the complete reaction to obtain the product. The preparation process has characteristics of simpleness, easy operation, extremely small three-waste generation, high yield, low cost, high product purity, and easy industrial production, wherein the yield is up to more than 90%. In the prior art, the piperazine citrate preparation process comprises adopting citric acid and piperazine hexahydrate as raw materials, adopting water as a solvent, and carrying out dissolving, salt forming, alcohol precipitation, centrifugation and drying, and has disadvantages of complex process, large wastewater generation and low yield. With the present invention, the disadvantages in the prior art are overcome.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis and relates to a preparation process of piperazine citrate. The invention also provides a piperazine citrate with high quality, safety and stability. Background technique [0002] Piperazine citrate (Piperazine Citrate), also known as Qushenling, is currently one of the more ideal anti-ascariasis drugs. The drug has the advantages of high curative effect, low toxicity, and easy usage, and is commonly used by medical personnel. The drug has the effect of paralyzing the muscles of roundworms, and its mechanism may be that piperazine exerts an anticholinergic effect at the neuromuscular junction of the worm body, blocks the excitatory effect of acetylcholine on the muscles of roundworms, or changes the permeability of the muscle cell membrane of the worm body to ions , affecting the transmission of nerve impulses; it can also inhibit the production of succinate, reduce the supply of energy, b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/027
Inventor 陈敏贺莲张静陈锋朱敏吴锋周江杨述罗玲唐清萍刘栋华
Owner KAMP PHARMA
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