Synthetic method of piperazidines drug intermediate

A synthesis method and intermediate technology, which are applied in the synthesis field of piperazine drug intermediates, can solve the problems of low product purity, harsh reaction conditions, complex synthesis route and the like, and achieve high product purity, simple route and simplified post-processing operation. Effect

Inactive Publication Date: 2015-03-11
SUZHOU JONATHAN NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, 1,4-N, the synthesis route of N-substituted piperazine compounds is complicated, the reaction conditions are harsh, and the product purity is low

Method used

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  • Synthetic method of piperazidines drug intermediate
  • Synthetic method of piperazidines drug intermediate
  • Synthetic method of piperazidines drug intermediate

Examples

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Comparison scheme
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Embodiment Construction

[0015] The present invention will be described in further detail below in conjunction with specific examples.

[0016] Step (1): Synthesis of bis(2-chloroethyl)methylamine hydrochloride.

[0017] Add 24 g (0.23 mol) diethanolamine to 35 mL CHCl 3 , stirred, slowly dropwise added 65mL (0.92mol) thionyl chloride and 40mL CHCl 3 The mixture was added dropwise in 1 hour, reacted for 2 hours, and removed excess thionyl chloride and CHCl under reduced pressure 3 , to obtain a light yellow solid, which was recrystallized from acetone to obtain bis(2-chloroethyl)methylamine hydrochloride as a white solid, 25.6 g, with a yield of 62%.

[0018] Step (2): Synthesis of 1-(3-chlorophenyl)piperazine hydrochloride.

[0019] 2.2 g (17.2 mmol) of 3-chloroaniline and bis(2-chloroethyl)methylamine hydrochloride (17.2 mmol) were dissolved in 20 mL of xylene. Heat to reflux for 24 hours. Extracted with dichloromethane, dried over anhydrous magnesium sulfate, and distilled off under reduced pr...

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Abstract

The invention discloses a synthetic method of a piperazidines drug intermediate. The synthetic method comprises the following steps: step one, reacting diethanol amine with thionyl chloride to prepare di(2-chloroethyl) methylamine hydrochloride; step two, reacting 3-chloroaniline with di(2-chloroethyl) methylamine hydrochloride to prepare 1-(3-chlorphenyl) piperazine hydrochlorid; step three, reacting 1-(3-chlorphenyl) piperazine hydrochloride with 1-bromine-3-chloropropane to prepare 1-(3-chlorphenyl)-4-(3-chloropropyl) piperazine hydrochloride. The line is simple, convenient and easy to perform, the aftertreatment operation is also greatly simplified, the reaction conditions are mild, and the product purity is high.

Description

technical field [0001] The invention relates to a method for synthesizing piperazine drug intermediates. Background technique [0002] Piperazine compounds are an important branch of heterocyclic compounds. 1, 4-N, N-substituted piperazine compounds are important drug intermediates in the synthesis of piperazine drugs such as etoperone, mebiprazole, aripiprazole, and nefazodone. In the prior art, the synthesis route of 1,4-N,N-substituted piperazine compounds is complex, the reaction conditions are harsh, and the product purity is low. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of piperazine drug intermediate, has solved the above-mentioned defect in the prior art. [0004] In order to achieve the above object, the technical scheme of the present invention is: a kind of synthetic method of piperazine drug intermediate, comprises the following steps: [0005] Step (1): the reaction of diethanolamine and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/073
CPCC07D295/073
Inventor 李卓才李苏杨
Owner SUZHOU JONATHAN NEW MATERIALS TECH
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