Method for preparing hydrochloric venlafaxine new crystal C

A technology of venlafaxine hydrochloride and its crystal form, which is applied in the preparation of venlafaxine hydrochloride and crystal form C of venlafaxine hydrochloride, and can solve the problems of high solvent recovery cost, low yield of crystal form C and solvent usage Achieving the effects of low cost, less solvent consumption and simple operation

Inactive Publication Date: 2008-06-25
ZHEJIANG APELOA JIAYUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention is aimed at the single solvent in the preparation method of the new crystal form C of venlafar hydrochloride, and the amount of solvent used is large, resulting in a low yield of the new crystal form C of venlafar hydrochlor

Method used

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  • Method for preparing hydrochloric venlafaxine new crystal C

Examples

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Example Embodiment

[0019] Example 1

[0020] Preparation of crude venlafaxine hydrochloride:

[0021] Add 100g of 1-[(2-amino)-1-(4-methoxyphenyl)ethyl]cyclohexanol with HPLC chromatographic purity greater than 96% into a 1000ml three-necked flask, then add 235g 36% formaldehyde and 145g 85% formic acid, heated and refluxed for reaction for 24 hours, cooled to 10°C, neutralized to pH 11 with 30% sodium hydroxide solution, extracted three times with 200ml×3 ethyl acetate, concentrated, and after concentration was completed with hydrogen chloride methanol Adjust the pH value of the solution to 2~3, and then concentrate the methanol, add 500ml ethyl acetate to crystallize, cool to 0~5℃ and filter with suction to obtain the crude venlafaxine hydrochloride.

[0022] Preparation of Venlafaxine Hydrochloride Form C:

[0023] At room temperature, add 1000g isopropanol and 100g crude venlafaxine hydrochloride into a 2000ml three-necked flask with condenser and thermometer, then raise the temperature to 60℃ u...

Example Embodiment

[0024] Example 2

[0025] Preparation of Venlafaxine Hydrochloride Form C:

[0026] At room temperature, add 600g of n-butanol and 100g of the crude venlafaxine hydrochloride prepared in Example 1 to a 1000ml three-necked flask with a condenser and a thermometer, and then raise the temperature to 80°C until the system is clear. After dissolving and cooling down to 0℃, crystallize for 1 hour. Stir continuously during the crystallization process. After crystallization, pass the SHZ-DC(III) circulating water vacuum pump (manufactured by Gongyi Yingyu Yuhua Instrument Factory) to control the load. The pressure is -0.06MPa for suction filtration; after suction filtration, the filter cake is washed with 50g n-butanol for 1 to 5 times and the suction filtration is continued. Manufactured by Shanghai Boxun Industrial Co., Ltd. Medical Equipment Factory), dried for 2-3 hours at a temperature of 60-80°C and a vacuum degree of 0.08Mp~0.1Mp to obtain 92.4g of venlafaxine hydrochloride crystal...

Example Embodiment

[0027] Example 3

[0028] Preparation of Venlafaxine Hydrochloride Form C:

[0029] At room temperature, into a 1000ml three-necked flask with a condenser and a thermometer, add 400g of ethyl acetate: methanol = 4:1 (weight ratio) mixed solvent, and 100g of the crude venlafaxine hydrochloride prepared in Example 1, Then increase the temperature to 80°C until the system is dissolved, and then cool down to 5°C to crystallize for 1.5 hours. Stir continuously during the crystallization process, and pass through the SHZ-DC(III) circulating water vacuum pump after crystallization. (Manufactured by Yingyu Yuhua Instrument Factory, Gongyi City) Control the negative pressure to -0.06MPa for suction filtration; after suction filtration, the filter cake is washed with a mixed solvent of 20g ethyl acetate:methanol=4:1 (weight ratio) for 1 to 5 times Continue suction filtration, the dried filtrate is recycled, and the filter cake is placed in a vacuum oven (model: DZF-6020, manufactured by Sha...

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Abstract

The invention relates to a preparation method for crystal form C of the venlafaxine hydrochloride, which comprises the following steps: A. dissolver; B. crystallization and pumping filtration; C. vacuum drying. The preparation method of the invention for crystal form C of the venlafaxine hydrochloride has simple operation, requires a small used amount of the solvents, requires a simple process of the solvent recycling and has low cost, and is beneficial to the large-scale industrialized production. The utilization of the preparation method of the invention can lead to the acquisition of the crystal form C of the venlafaxine hydrochloride and the purity of the products is high and meets the requirement of the drug specification; the products are easy to be stored, the resistance can be kept stable for a long time and the yield of the products is high.

Description

technical field [0001] The invention relates to a preparation method of venlafax hydrochloride, in particular to a preparation method of a new crystal form C of venlafax hydrochloride; it belongs to the field of medicine and chemical industry. Background technique [0002] Venlafaxine hydrochloride, its chemical name is 1-[(2-dimethylamino)-1-(4-methoxyphenyl)ethyl]cyclohexanol hydrochloride. Venlafaxine hydrochloride is an antidepressant drug that exerts antidepressant effects through the reuptake of norepinephrine and serotonin, and is an alternative product to tricyclic antidepressants and selective reuptake inhibitors . [0003] The preparation method of Chinese patent application (200610050889.X) venlafaxine, the method comprises the following steps: the first step is raw material with 4-methoxyphenylacetonitrile, in lye, by phase transfer catalyst effect, with cyclohexane Ketone condensation to obtain 1-[cyano-1-(4-methoxyphenyl) ethyl] cyclohexanol; the second step ...

Claims

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Application Information

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IPC IPC(8): C07C217/74C07C213/10
Inventor 张拥军吴朝刚朱勇华章中华
Owner ZHEJIANG APELOA JIAYUAN PHARMA
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