Preparation method of piperazine and own derivatives

Abstract

The invention provides a method for preparing piperazine and own derivatives. Specifically, the method is characterized by taking glycol as the raw material and ensuring the aqueous solution of glycol to react in a reactor in the presence of a catalyst in hydrogen and ammonia to obtain the mixture of piperazine and own derivatives. The method has the advantages of low-price and easily obtained raw material, high conversion rate, easy preparation of the catalyst, stable activity, long service life, high product selectivity, etc.

Description

technical field [0001] The invention relates to the field of chemical drug synthesis, more specifically, relates to a method for preparing piperazine and derivatives thereof by using ethylene glycol as a raw material. Background technique [0002] Piperazine is an important organic chemical intermediate. It is widely used in medicine, pesticides, dyes and surfactants and other fields. Piperazine and its derivatives can be used as raw materials to synthesize drug intermediates such as lomefloxacin hydrochloride, sparfloxacin and anthrafloxacin. The research on piperazine abroad is relatively extensive, and there are hundreds of patents related to it. According to the different synthetic methods of the raw materials used, there are mainly the following: JP4911712 and JP74125375 etc. have reported the process route of preparing piperazine by hydrogenation and cyclization of N-β-hydroxyethylethylenediamine as raw material. This method uses copper, chromium Oxides of metals su...

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Problems solved by technology

According to the different synthetic methods of the raw materials used, there are mainly the following: JP4911712 and JP74125375 etc. have reported the process route of preparing piperazine by hydrogenation and cyclization of N-β-hydroxyethylethylenediamine as raw material. This method uses copper, chromium Oxides of metals such as manganese and manganese are catalysts, which have the advantages of few by-products and higher yields, and the highest yield can reach more than 90%, but its technology is intermittent production, and the production efficiency is low; patents such as US368219 have reported that two Ethylene triamine is a process for preparing piperazine by deamination under high temperature and catalyst action. The yield of this method is relatively high, which can reach about 80%, but the raw material price is high, which restricts the industrialization of this process; EP16325304 and other reports Using aminoethanol as a raw material, the process of synthesizing piperazine under the action of high temperature and high pressure and a catalyst co-produces ethylenediamine, but the piperazine yield of this route is low, between 15-25%; Diamine is used as raw material and KZSM-5 zeolite molecular sieve is used as a catalyst to produce piperazine by-product triethylenediamine. The total yield of this process is relatively high, but the service life of the catalyst does not meet the requirements of industrialization.

In addition, BASF, Nobel, etc. have reported the patent of extracting piperazine from the by-products of ethylenediamine and diethylenetriamine, but because the content of piperazine in such products is generally low, the extraction is relatively difficult

The preparation of other piperazine derivatives also generally has the problem of high cost or short catalyst life, so it is necessary to carry out research on new piperazine synthesis processes

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