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Preparation method of high-purity Z-type flupentixol and Z-type flupentixol decanoate

A technology for flupentixol decanoate and flupentixol is applied in the field of preparation of high-purity Z-type flupentixol and Z-type flupentixol decanoate, and can solve the problems of complicated operation, low purity and the like , to achieve the effect of high curative effect, high purity and high economic benefit

Pending Publication Date: 2022-03-01
JIANGSU TOHOPE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many literature reports on the preparation methods of flupenthixol. The ratio of (Z)-type isomer and (E)-type isomer in the prepared flupenthixol is mostly close to 1:1. Although (Z)-type isomer can be )-flupenthixol is isolated from the mixture, but the operation is cumbersome and the purity is low (mostly 95% purity)

Method used

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  • Preparation method of high-purity Z-type flupentixol and Z-type flupentixol decanoate
  • Preparation method of high-purity Z-type flupentixol and Z-type flupentixol decanoate
  • Preparation method of high-purity Z-type flupentixol and Z-type flupentixol decanoate

Examples

Experimental program
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Effect test

Embodiment 1

[0036] The preparation method of high-purity Z-type flupenthixol comprises the following steps:

[0037] S1. Take 1mol flupenthixol and 1700ml acetone, stir and dissolve after mixing, pass 1.2mol hydrogen chloride gas into the mixed solution, let it stand at room temperature for 2h, then carry out suction filtration to the mixed solution, collect the product, and get flupenthix hydrochloride tons of crude products;

[0038] S2. Mix the crude product of flupenthixol hydrochloride with 200ml of methanol, heat to 40°C and stir to dissolve, then add 600ml of diethyl ether, stir and gradually lower to room temperature, make the mixed liquid crystallize, filter, and collect the product to obtain flupenthixol hydrochloride Z-type Ton;

[0039] S3. Mix Z-type flupentixol hydrochloride with 600ml of methanol and 100ml of water, stir to dissolve, then add 70g of 90% potassium hydroxide aqueous solution, place the reaction vessel in a constant temperature water bath heater, heat to 45°C...

Embodiment 2

[0047] The difference between this example and Example 1 is that in step S1, 1 mol of flupenthixol and 1700 ml of acetone are taken, stirred and dissolved after mixing, 1.3 mol of hydrogen chloride gas is passed into the mixed solution, and left to stand at room temperature for 2 hours, and then mixed The liquid was subjected to suction filtration, and the product was collected to obtain the crude product of flupenthixol hydrochloride.

[0048] The prepared Z-type flupenthixol was detected by liquid chromatography (reference substance external standard method), and its purity was 99.8012%.

Embodiment 3

[0050] The difference between this example and Example 1 is that in step S1, 1 mol of flupenthixol and 1700 ml of acetone are taken, mixed, stirred and dissolved, 1.4 mol of hydrogen chloride gas is passed into the mixed solution, and left to stand at room temperature for 2 hours, and then mixed The liquid was subjected to suction filtration, and the product was collected to obtain the crude product of flupenthixol hydrochloride.

[0051] The prepared Z-type flupenthixol was detected by liquid chromatography (reference substance external standard method), and its purity was 99.8556%.

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Abstract

The invention discloses a preparation method of high-purity Z-type flupentixol and a preparation method of Z-type flupentixol decanoate. The invention relates to a preparation method of high-purity Z-type flupentixol, which comprises the following steps: dissolving flupentixol in an organic solvent, introducing hydrogen chloride gas into the solution according to the molar ratio of flupentixol to hydrogen chloride of 1: (1.2-1.5), crystallizing and carrying out suction filtration to obtain a flupentixol hydrochloride crude product; the method comprises the following steps: mixing a flupentixol hydrochloride crude product with an organic solvent, heating and dissolving, adding diethyl ether, stirring, cooling, crystallizing, and filtering to obtain the Z-type flupentixol hydrochloride, the preparation method comprises the following steps: mixing Z-type flupentixol hydrochloride, methanol and water, adding a potassium hydroxide aqueous solution, carrying out heating reaction, and then carrying out reduced pressure distillation concentration to obtain a concentrate; and mixing the concentrate, water and toluene, heating, separating each phase, collecting an organic phase, evaporating the solvent, and concentrating into a residue, thereby obtaining the Z-type flupentixol. The preparation method of the high-purity Z-type flupentixol has the advantage that the high-purity Z-type flupentixol can be obtained.

Description

technical field [0001] The application relates to the field of preparation of Z-type flupenthixol decanoate, more specifically, it relates to the preparation method of high-purity Z-type flupenthixol and Z-type flupentixol decanoate. Background technique [0002] Flupenthixol decanoate, the chemical name is (Z)-2-[4-[3-(2-trifluoromethylthioxanthene-9-ylidene)-propyl]piperazin-1-yl]ethyl Acyldecanoate, trade name Fulansu, developed by the Danish Lundbeck Pharmaceutical Company, currently its injection is mainly marketed in the UK, Canada, Belgium and other places. Flupenthixol decanoate is a long-acting preparation of flupenthixol, an antagonist of dopamine D2 receptors and 5-hydroxytryptamine (5-HT) receptors, and is used for various acute and chronic schizophrenia. [0003] Flupenthixol consists of a mixture of two geometric isomers Z and E. The Z isomer of flupenthixol, hereinafter also referred to as (Z)-flupenthixol, is a more active isomer, which is currently prepare...

Claims

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Application Information

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IPC IPC(8): C07D335/20
CPCC07D335/20C07B2200/09
Inventor 龚利锋邵仲昆戴国新陆惠刚钱栋
Owner JIANGSU TOHOPE PHARMA
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