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Novel preparation method of 1-[((2-hydroxyethyoxyl)ethyoxyl)ethyl]piperazine hydrochloride

A technology of hydroxyethoxy and ethoxy, applied in the field of preparing pharmaceutical intermediate 1-[ethoxy)ethyl]piperazine hydrochloride, can solve the problems of long route, time-consuming, difficult to use and the like

Inactive Publication Date: 2019-03-01
WUXI QIANHAO BIOPHARMA
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  • Summary
  • 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 of 1-[((2-hydroxyethyoxyl)ethyoxyl)ethyl]piperazine hydrochloride

Examples

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example 1

[0012] 100 grams (1.2mol) of anhydrous piperazine and 240 grams (1.5mol) of piperazine dihydrochloride were heated to 120 degrees Celsius, and 160 grams (1.2mol) of 1-[((2-chloroethoxy) ethyl Oxygen) ethanol, continue heating and stirring after adding, heat up to 136-140 degrees Celsius, keep for 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 off 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 a white solid 1-[((2-hydroxyethoxy )ethoxy)ethyl]piperazine hydrochloride; the solid content is already abo...

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Abstract

The invention discloses a practical synthesis method for preparing an important medicine raw material 1-[((2-hydroxyethyoxyl)ethyoxyl)ethyl]piperazine hydrochloride. In the presence of a proper solvent or in the absence of a solvent, piperazine and 1-[((2-chloroethyoxyl)ethyoxyl)ethanol are stirred to react at 100-150 DEG C; 1-[((2-hydroxyethyoxyl)ethyoxyl)ethyl]piperazine hydrochloride is directly obtained with high yield without protection of one amino of piperazine.

Description

technical field [0001] The invention provides an economical and practical new method for preparing pharmaceutical intermediate 1-[((2-hydroxyethoxy)ethoxy)ethyl]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 dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/088
CPCC07D295/088Y02P20/55
Inventor 彭海燕
Owner WUXI QIANHAO BIOPHARMA
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