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Process for preparing N-benzyl piperazine

A technology of benzylpiperazine and piperazine, which is applied in the field of preparation of N-benzylpiperazine, can solve the problems of low yield, complicated operation and low product purity, and achieves a high yield, simple operation and high purity. Effect

Inactive Publication Date: 2009-07-15
亚邦投资控股集团有限公司
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Problems solved by technology

In addition, the main reaction will have some side reactions at the same time. In order to prevent the side reactions, it is often necessary to use an excessive amount or even several times the amount of piperazine to participate in the reaction, so that post-treatment will be carried out after the reaction. Unreacted piperazine and the target product N-benzylpiperazine is separated, the operation is more complicated, the product purity is low, and the yield is very low, which can only reach 60-70%.

Method used

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  • Process for preparing N-benzyl piperazine

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Embodiment approach

[0019] In a 500ml reaction bottle, drop 25.8g (0.3mol) of piperazine and 100ml of solvent anhydrous methanol, stir and dissolve, then drop into the catalyst aniline hydrochloride, heat up to 50 degrees, drop 38g (0.3mol) of benzyl chloride, about Add dropwise in half an hour. Keep the temperature at 50°C for 3 hours, cool to normal temperature, reduce the pressure to 15mmhg, and evaporate to remove the solvent methanol. Then add NaOH solution, adjust the pH value to 13, and extract twice with ethyl acetate, each with 50 ml of ethyl acetate. Distill the extract under normal pressure, reduce the pressure to 2.5 mmhg, and collect fractions at 120—124°C by distillation to finally obtain 50.5 g of the target product, N-benzylpiperazine, with a yield of 95.5% and a purity of 99.2%.

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Abstract

The preparation method of N-benzylpiperazine is that piperazine and benzyl halide react under catalyst conditions to generate N-benzylpiperazine, piperazine is dissolved in a solvent, and nitrogen-containing amine salt is dropped into as a catalyst, at 0-100 Add dropwise benzyl halide and piperazine at ℃ to react, keep warm for 0.5-24 hours after the reaction, evaporate the solvent under reduced pressure, add lye to strong alkalinity, extract with extractant, and then distill and rectify to obtain the finished product. The invention has the advantages of minimizing the post-treatment procedure after the reaction, simple operation, high purity of the target product, which can reach more than 99%, and the yield can reach more than 95%.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular N-benzylpiperidine, an intermediate of pharmaceutical products such as rifamycin for treating tuberculosis infection, dopamine for treating and preventing neuropsychological diseases, and trimetazidine for relaxing blood vessels. The preparation method of oxazine. Background technique [0002] N-benzyl piperazine (N-benzyl piperazine) is an important nitrogen-containing heterocyclic compound and a pharmaceutical intermediate. Its derivatives can be made into a variety of pharmaceutical products, such as rifamycin for the treatment of tuberculosis infection , dopamine for the treatment and prevention of neuropsychological diseases, trimetazidine for dilating blood vessels, and antiallergic drug pyridazinone, etc. The current preparation method of N-benzylpiperazine is formed by condensation of piperazine and benzyl halide under the action of a catalyst. Commo...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/03
Inventor 张俭郑小刚
Owner 亚邦投资控股集团有限公司
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