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
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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 hydrochloride; the cost of recovering the solvent is high, and the pressure on environmental protection is high. The invention provides a method for preparing new crystal form C of Venlafax hydrochloride with low production cost and high product purity and yield

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  • Method for preparing hydrochloric venlafaxine new crystal C

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Embodiment 1

[0020] Preparation of crude venlafaxine hydrochloride:

[0021] The 1-[(2-amino)-1-(4-methoxyphenyl) ethyl] cyclohexanol that 100g HPLC chromatographic purity is greater than 96% is added in the there-necked bottle of 1000ml, then adds the formaldehyde of 235g 36% and 145g 85% formic acid, heat up and reflux for 24 hours, cool down to 10°C, neutralize with 30% sodium hydroxide solution to pH 11, extract with 200ml×3 ethyl acetate three times, concentrate, and use hydrogen chloride methanol after concentration Adjust the pH value of the solution to 2-3, then concentrate the methanol, add 500ml of ethyl acetate for crystallization, cool down to 0-5°C and suction filter to obtain the crude venlafaxine hydrochloride.

[0022] Preparation of Venlafaxine Hydrochloride Form C:

[0023] At room temperature, add 1000g of isopropanol and 100g of crude venlafaxine hydrochloride to a 2000ml three-neck flask with a condenser tube and a thermometer, then raise the temperature to 60°C until...

Embodiment 2

[0025] Preparation of Venlafaxine Hydrochloride Form C:

[0026] At room temperature, add 600 g of n-butanol and 100 g of the crude venlafaxine hydrochloride prepared in Example 1 to a 1000 ml three-necked flask with a condenser tube and a thermometer, then raise the temperature to 80° C. until the system dissolves, After the dissolution, the temperature was lowered to 0°C for crystallization for 1 hour. During the crystallization process, it was stirred continuously. 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 to continue suction filtration, and the filtrate after draining is recycled, and the filter cake is placed in a vacuum oven (model: DZF-6020, (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 of 0.08Mp to 0.1Mp to obtain 92.4g of the new crystal form C of venlafax hydrochloride. rate gre...

Embodiment 3

[0028] Preparation of Venlafaxine Hydrochloride Form C:

[0029] At room temperature, in the there-necked flask that 1000ml has condenser tube and thermometer, add the mixed solvent of 400g ethyl acetate: methyl alcohol=4: 1 (weight ratio), the venlafaxine hydrochloride crude product prepared with 100g embodiment 1, Then raise the temperature to 80°C until the system is dissolved, and then cool down to 5°C for crystallization for 1.5 hours. Stir continuously during the crystallization process, and then pass the SHZ-DC(III) circulating water vacuum pump after the crystallization (Manufactured by Yingyu Yuhua Instrument Factory in Gongyi City) Control the negative pressure to be -0.06MPa and carry out suction filtration; after suction filtration, the filter cake is washed 1 to 5 times with a mixed solvent of 20g ethyl acetate:methanol=4:1 (weight ratio) Continue suction filtration, recycle the filtrate after drying, put the filter cake in a vacuum oven (model: DZF-6020, manufact...

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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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