Preparation method of piperazine phosphate

A technology of piperazine phosphate and phosphoric acid, applied in organic chemistry and other directions, can solve the problems of unclear mechanism of action, large environmental pollution, complicated process and other problems, and achieve the effects of low equipment requirements, low equipment investment and simple process

Inactive Publication Date: 2014-02-26
江苏黄河药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, it also has anthelmintic effect on pinworms, but the mechanism of action is not yet clear
[0003] At present, there is no relevant patent protection for the preparation method of piperazine phosphate in China. The traditio

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 3000 ml of 97.97 g of phosphoric acid in ethanol to a 10000 ml reaction kettle, and heat to 45° C.; dropwise add 3000 ml of 86.14 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. 166.5 g of piperazine phosphate was obtained, the content was 99.3%, and the yield was 90.4%.

Embodiment 2

[0024] Add 97.97g of phosphoric acid in 3500ml of dichloromethane solution to a 10000ml reactor, and heat to 60°C; add dropwise 86.14g of anhydrous piperazine in 4000ml of dichloromethane solution into the reactor. The dropwise addition time was 50 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. 168.5 g of piperazine phosphate was obtained, the content was 99.7%, and the yield was 91.5%.

Embodiment 3

[0026] Add 4000ml of ethanol solution of 97.97g phosphoric acid in a 10000ml reactor, heat to 60°C; add dropwise 3000ml of ethanol solution of 86.14g anhydrous piperazine into the reactor. 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. 170.2 g of piperazine phosphate was obtained, the content was 99.6%, and the yield was 92.4%.

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Abstract

The invention relates to a preparation method of piperazine phosphate. The method includes: fully dissolving phosphoric acid and anhydrous piperazine in an organic solvent, and conducting filtering, salifying the two substances in a reaction kettle under suitable reaction conditions, and after complete reaction, carrying out cooling crystallization, centrifugation, washing, and vacuum drying, thus obtaining the piperazine phosphate. The method provided by the invention employs fewer organic solvent, achieves a yield up to over 90%, the product has high purity, also the process is simple, the operation is easy, the cost is greatly lowered, and the method is easy for industrial production. The piperazine phosphate provided by the invention is often used for treating children's ascaris and pinworm infection.

Description

technical field [0001] The invention relates to a preparation method of piperazine salt, in particular to a preparation method of piperazine phosphate. The invention also provides a piperazine phosphate with good stability and high quality. The synthesized piperazine phosphate is mainly used for medicine. Background technique [0002] Piperazine phosphate is also known as piperazine phosphate or piperazine phosphate monohydrate, the chemical formula is C 4 h 10 N 2 h 3 PO 4 h 2 O, molecular weight 202.15. Piperazine phosphate pagoda sugar with piperazine phosphate as the main component is a traditional anthelmintic drug and one of the ideal anthelmintic drugs at present. The medicine has the advantages of high curative effect, low toxicity, easy usage and the like. Piperazine phosphate has the effect of paralyzing roundworms, and the mechanism of expelling roundworms may be that piperazine exerts an anticholinergic effect at the neuromuscular junction of the worm bod...

Claims

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Application Information

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IPC IPC(8): C07D295/027C07D295/023
CPCC07D295/027C07D295/023
Inventor 葛海涛王晓磊苏恺琪唐俊
Owner 江苏黄河药业股份有限公司
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