Novel preparation method for 1-(2-hydroxyethyl)piperazine hydrochloride

A technology of hydroxyethyl and hydrochloride, applied in the field of preparing pharmaceutical intermediate 1-piperazine hydrochloride, can solve the problems of low total yield, difficult to use, time-consuming and the like

Inactive Publication Date: 2019-02-26
南京海燕生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These traditional process routes are long, time-consuming, and the total yield is low. They have great defects in industrial production and are difficult to adopt.

Method used

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  • Novel preparation method for 1-(2-hydroxyethyl)piperazine hydrochloride

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example 1

[0012] Heat 100 grams (1.2mol) of anhydrous piperazine and 240 grams (1.5mol) of piperazine dihydrochloride to 120 degrees Celsius, add dropwise 110 grams (1.2mol) of 2-chloroethanol, continue heating and stirring after adding, and heat up To 136-140 degrees Celsius, keep 1 hour, stop heating after TLC shows that the reaction is complete. When the temperature drops to 80 degrees Celsius, add 500 milliliters of 95% ethanol, cool overnight in the refrigerator, filter and recover piperazine dihydrochloride the next day, wash the filter cake fully with a small amount of ethanol, combine the filtrates, and add 30% sodium hydroxide solution 200 grams of alkalization, filtered out insoluble inorganic salts; concentrated to remove the solvent, extracted the residue with ethyl acetate, passed through dry hydrogen chloride gas, filtered and dried to obtain white solid 1-(2-hydroxyethyl)piperazine Hydrochloride; the solid content is already above 98%. After one recrystallization with 90...

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Abstract

The invention elaborates a practical synthetic method for preparing an important medical pharmaceutical raw material 1-(2-hydroxyethyl)piperazine hydrochloride. Reaction can be performed on piperazinehydrochloride and 2-chloroethanol through stirring under 100-150 DEG C under a suitable solvent or solvent-free condition; and 1-(2-hydroxyethyl)piperazine hydrochloride can be directly obtained withhigh yield without protecting an amino of piperazine.

Description

technical field [0001] The invention provides an economical and practical new method for preparing pharmaceutical intermediate 1-(2-hydroxyethyl)piperazine hydrochloride. Background technique [0002] Piperazine is an important component of many drugs. It is a six-membered heterocyclic ring containing two nitrogen atoms in the molecule. It is an ideal structural unit of nitrogen-rich heterocyclic compounds. It has the characteristics of high formation enthalpy and good thermal stability. In recent years, the application of piperazine compounds in organic synthesis and medicine has attracted widespread attention in the field of organic chemistry and pharmacy. Compared with traditional organic drugs, the piperazine ring has a symmetrical structure with better nitrogen balance. The introduction of piperazine rings in drug synthesis can be used as drug synergistic groups to improve the pharmacokinetic properties of drugs and increase the biological activity of drugs; compounds c...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07D295/088
CPCC07D295/088
Inventor不公告发明人
Owner南京海燕生物医药科技有限公司