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A kind of preparation method of flupenthixol hydrochloride

A technology for flupentixol hydrochloride and flupentixol hydrochloride is applied in the field of preparation of flupentixol hydrochloride, can solve the problems of low yield, complicated procedures, and is not easy to industrialize production, and achieves high yield and high product purity. , the effect of fewer steps

Active Publication Date: 2018-03-27
MITSUBISHI PHARMA GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process is complicated, the yield is low, and it is not easy to realize industrial production

Method used

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  • A kind of preparation method of flupenthixol hydrochloride

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Embodiment 1

[0026] Embodiment 1: a kind of embodiment of the preparation method of 10-[3-(EZ)-dimethylaminopropyl group]-2-trifluoromethylthioxanthene of the present invention (acetic anhydride and 10-hydroxyl-10 The molar ratio of -(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene is about 1.46:1)

[0027] Put 3.67kg of 10-hydroxy-10-(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene and 35kg of tetrahydrofuran into the reaction kettle, add 1.7kg of acetic anhydride at room temperature for reaction, and concentrate under reduced pressure after the reaction is completed The reaction solution, the residue was dissolved in 40 kg of ethyl acetate, then washed with 40 kg of saturated sodium bicarbonate solution, the ethyl acetate layer was dried and concentrated under reduced pressure to obtain 10-[3-(EZ)-dimethylaminopropyl]- 2-trifluoromethylthioxanthene, its Z-type product content is 48%, yield: 100%. 10-[3-(EZ)-dimethylaminopropyl]-2-trifluoromethylthioxanthene Z type content dete...

Embodiment 2

[0028] Embodiment 2: a kind of embodiment of the preparation method of 10-[3-(EZ)-dimethylaminopropyl group]-2-trifluoromethylthioxanthene of the present invention (acetic anhydride and 10-hydroxyl-10 The molar ratio of -(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene is 1:1)

[0029] Put 3.22kg of 10-hydroxy-10-(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene and 35kg of acetone into the reaction kettle, add 1.02kg of acetic anhydride at room temperature for reaction, and concentrate under reduced pressure after the reaction is completed The reaction solution, the residue was dissolved in 40 kg of ethyl acetate, then washed with 40 kg of saturated sodium bicarbonate solution, the ethyl acetate layer was dried and concentrated under reduced pressure to obtain 10-[3-(EZ)-dimethylaminopropyl]- 2-trifluoromethylthioxanthene, its Z-type product content is 46%, yield: 100%. 10-[3-(EZ)-dimethylaminopropyl]-2-trifluoromethylthioxanthene Z type content determination method...

Embodiment 3

[0030] Embodiment 3: a kind of embodiment of the preparation method of 10-[3-(EZ)-dimethylaminopropyl group]-2-trifluoromethylthioxanthene of the present invention (acetic anhydride and 10-hydroxyl-10 The molar ratio of -(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene is 4:1)

[0031]Put 3.22kg of 10-hydroxy-10-(3-dimethylaminopropyl)-2-trifluoromethylthioxanthene and 35kg of tetrahydrofuran into the reaction kettle, add 4.08kg of acetic anhydride at room temperature for reaction, and concentrate under reduced pressure after the reaction is completed The reaction solution, the residue was dissolved in 40 kg of ethyl acetate, then washed with 40 kg of saturated sodium bicarbonate solution, the ethyl acetate layer was dried and concentrated under reduced pressure to obtain 10-[3-(EZ)-dimethylaminopropyl]- 2-trifluoromethylthioxanthene, its Z-type product content is 49%, yield: 100%. 10-[3-(EZ)-dimethylaminopropyl]-2-trifluoromethylthioxanthene Z type content determination...

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Abstract

The invention provides a preparation method of flupentixol dihydrochloride, which comprises the following steps: reacting and dehydrating 10-hydroxy-10-(3-dimethylaminopropyl)-2-trifluoromethyl thioxanthene and sulfoxide chloride or acetic anhydride to prepare high-content Z-type 10-[3-(EZ)-dimethylaminopropyl]-2-trifluoromethyl thioxanthene, reacting with N-hydroxyethyl piperazidine to prepare flupentixol base, and finally, introducing sufficient hydrochloric acid gas into the flupentixol base to prepare the high-content Z-type flupentixol dihydrochloride. The method has the advantages of fewer steps, high yield and high product purity, is simple to operate, and does not use any extremely toxic substance to pollute the environment. The Z-type flupentixol dihydrochloride content in the flupentixol dihydrochloride prepared by the method is 42-52%, and conforms to the quality standard specification for flupentixol dihydrochloride in European Pharmacopoeia.

Description

technical field [0001] The invention relates to a preparation method of flupenthixol hydrochloride, in particular to a preparation method of flupenthixol hydrochloride with a medicinal Z-type content of 42% to 52%. Background technique [0002] Flupenthixol hydrochloride is the dihydrochloride of flupenthixol, and its combination compound preparation with melitracen hydrochloride (trade name: Deanxit) is used to treat depression, anxiety and severe tension. The structural formula of flupenthixol is as follows: [0003] [0004] The quality standard of flupenthixol hydrochloride recorded in the European Pharmacopoeia stipulates that the content of the Z-isomer should be in the range of 42.0% to 52.0%. Acceptance is a very difficult thing. There are mainly two kinds of existing preparation technologies, one is to separate and purify type Z and type E, and mix the two isomers in a certain proportion to prepare flupentixol hydrochloride medicinal product; the other is to co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D335/20
CPCC07D335/20
Inventor 梁峰石杰
Owner MITSUBISHI PHARMA GUANGZHOU
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