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Preparation method of 1-(2,3-dichlorophenyl) piperazine hydrochloride

A technology of dichlorophenyl and hydrochloride, applied in the field of chemistry, can solve the problems of long reaction time, low yield and high cost, and achieve the effects of simple operation, high yield and low cost

Inactive Publication Date: 2014-06-18
江西华龙化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first method is economical and easy to obtain raw materials, but the reaction time is long, the yield is low, and a large amount of acid waste gas and waste liquid is produced; the second method requires precious metal catalysts, or the target product can be obtained through multi-step reactions, resulting in low yield ,higher cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: In a 500L electric heating reaction kettle, add 100 kg of 2,3-dichloroaniline, turn on the stirring, turn on the electric heating to raise the temperature of the liquid in the kettle to 100°C and keep the temperature at 100°C, divide 5 batches of 110 Pour two kilograms of bis-(2-chloroethyl)amine hydrochloride solid into the reaction kettle, continue to heat up to 120°C, keep the temperature for 34 hours, stop heating, exhaust the tail gas, add 200 kilograms of n-butanol, reflux and stir for 1 hour, Cooling and crystallization, centrifugation, the crude product was refined with 300 kg of methanol, after cooling and crystallization, centrifugation and drying, 98.0 kg of 1-(2,3-dichlorophenyl)piperazine hydrochloride was obtained, purity (HPLC): 99.62 %, yield 59.5%.

Embodiment 2

[0018] Example 2: In a 500L electric heating reactor, add 100 kg of 2,3-dichloroaniline, turn on the stirring, turn on the electric heating to raise the temperature of the liquid in the kettle to 100°C and keep the temperature at 100°C, divide 7 batches of 165 kg Put the bis-(2-chloroethyl)amine hydrochloride solid into the reaction kettle, continue to heat up to 160°C, keep the temperature for 12 hours, stop heating, exhaust the tail gas, add 230 kg of n-butanol, reflux and stir for 1 hour, and cool down Crystallization, centrifugation, the crude product was refined with 300 kg of methanol and water (10:1) mixed solvent, and after cooling, crystallization, centrifugation, and drying, 1-(2,3-dichlorophenyl)piperazine hydrochloride 105.5 kg, purity (HPLC): 99.58%, yield 64.0%.

Embodiment 3

[0019] Example 3: In a 500L electric heating reactor, add 100 kg of 2,3-dichloroaniline, turn on the stirring, turn on the electric heating to raise the temperature of the liquid in the kettle to 100°C and keep the temperature at 100°C, divide 8 batches of 200 kg Put the bis-(2-chloroethyl)amine hydrochloride solid into the reaction kettle, continue to heat up to 200°C, keep the temperature for 4 hours, stop heating, exhaust the tail gas, add 250 kg of n-butanol, reflux and stir for 1 hour, cool down Crystallization, centrifugation, the crude product was refined with 350 kg of methanol and water (10:1) mixed solvent, and after cooling, crystallization, centrifugation, and drying, 1-(2,3-dichlorophenyl)piperazine hydrochloride 108.2 kg, purity (HPLC): 99.67%, yield 65.6%.

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PUM

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Abstract

The invention discloses a preparation method of 1-(2,3-dichlorophenyl) piperazine hydrochloride, which is characterized by comprising the following steps: carrying out cyclization reaction 2,3-dichloroaniline as a raw material with bis(2-chloroethyl) amine hydrochloride, wherein the charging temperature is 90-120 DEG C, and the reaction temperature is 120-220 DEG C; and treating reaction liquid after the reaction by using an after-treatment solvent, so as to obtain a coarse product, and carrying out refining on the coarse product so as to obtain a refining after-treatment solvent so as to obtain a product with purity meeting the requirement. The mass ratio of the 2,3-dichloroaniline to the bis(2-chloroethyl) amine hydrochloride is 1:(0.8-2.0), and the after-treatment solvent and the refining after-treatment solvent are protonic solvents. According to the method, the yield is high, waste liquid is relatively little, the cost is low, the purity (HPLC (High Performance Liquid Chromatography)) is up to more than 99.5%, and the yield is up to more than 59.5%; and the method is suitable for industrial production of the 1-(2,3-dichlorophenyl) piperazine hydrochloride.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a preparation method of 1-(2,3-dichlorophenyl)piperazine hydrochloride Background technique [0002] 1-(2,3-dichlorophenyl)piperazine hydrochloride is the main intermediate of aripiprazole, an atypical antipsychotic, and its preparation method can be divided into two types from the raw materials and reaction types: one is based on 2 , 3-dichloroaniline and bis-(2-chloroethyl)amine hydrochloride are prepared by cyclization reaction in different solvents; the other is prepared by condensation reaction of different halogenated benzenes and piperazine, including 2,3-dichlorobromobenzene is directly condensed with piperazine and 2,6-dichloronitrobenzene is condensed with anhydrous piperazine and then prepared through multi-step reaction. The first method is economical and easy to obtain raw materials, but the reaction time is long, the yield is low, and a large amount of acid waste gas and w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/073
Inventor 李铭东杨龙马红蓝华军徐泽民
Owner 江西华龙化工有限公司
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