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Fluoxertine hydrochloride compound and new preparation method thereof

A technology of fluoxetine hydrochloride and compounds, which is applied in the field of fluoxetine hydrochloride compounds, can solve the problems of low purity of fluoxetine hydrochloride, achieve the effects of reducing toxic and side effects, reducing residues, and improving product quality

Inactive Publication Date: 2013-12-11
HAINAN MEIDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to overcome the defect of low purity of fluoxetine hydrochloride prepared by the prior art, the invention provides a method for refining fluoxetine hydrochloride compound, in order to improve the purity of fluoxetine hydrochloride, reduce the residue of toxic solvents, and through the method of the present invention The purification method also helps to improve the quality of preparation products, reduce toxic and side effects, and is suitable for large-scale industrial production

Method used

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  • Fluoxertine hydrochloride compound and new preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Get 10g of fluoxetine hydrochloride crude drug with a long production date (manufacturer Shanxi Qianyuan Pharmaceutical Co., Ltd., batch number 20090501), and the purity measured by high performance liquid chromatography is 94.48%. Dissolve this fluoxetine hydrochloride raw material in 40ml acetone, fully stir, make it dissolve completely, filter to remove insoluble impurity, collect filtrate once.

[0054] Add 0.2 g of activated carbon to the primary filtrate, stir and adsorb at 40°C for 15 minutes, filter the deactivated carbon, collect the secondary filtrate, and concentrate under reduced pressure at 60°C.

[0055] Add 10g of alumina to the above-mentioned concentrated filtrate, stir evenly, evaporate the solvent and add to the upper end of the preparative chromatographic column, and then use the preparative chromatographic column to separate and purify, wherein the mobile phase used in the chromatographic column has a volume ratio of 2: 5:2 mixed solution of acetoni...

Embodiment 2

[0061] Take 10 g of expired fluoxetine hydrochloride raw material (manufacturer Shanxi Qianyuan Pharmaceutical Co., Ltd., batch number 20081201), and the purity measured by high performance liquid chromatography is 92.24%. Dissolve this fluoxetine hydrochloride raw material in 50ml ethanol, fully stir, make it dissolve completely, filter to remove insoluble impurity, collect filtrate once.

[0062] Add 0.3 g of alumina to the primary filtrate, stir and adsorb at 35°C for 10 minutes, filter the de-alumina, collect the secondary filtrate, and concentrate under reduced pressure at 55°C.

[0063] Add the above-mentioned concentrated filtrate to the upper end of the preparative chromatographic column, and then use the preparative chromatographic column to separate and purify the filtrate, wherein the mobile phase used in the chromatographic column is a mixed solution of acetonitrile:methanol:water with a volume ratio of 2:5:2 , the flow rate is 2ml / min, the stationary phase filler ...

Embodiment 3

[0069] Take 10 g of fluoxetine hydrochloride crude product prepared according to US2004102561A1, and the purity is 93.28% as measured by high performance liquid chromatography. Dissolve this fluoxetine hydrochloride raw material in the mixed solvent of 60ml ethanol and methanol, fully stir, make it dissolve completely, filter to remove insoluble impurity, collect filtrate once.

[0070] Add 0.2 g of A-type molecular sieve to the primary filtrate, stir and adsorb at 35°C for 15 minutes, filter and remove the molecular sieve, collect the secondary filtrate, and concentrate under reduced pressure at 60°C.

[0071] Add the above-mentioned concentrated filtrate to the upper end of the preparative chromatographic column, and then use the preparative chromatographic column to separate and purify the filtrate, wherein the mobile phase used in the chromatographic column is a mixed solution of acetonitrile:methanol:water with a volume ratio of 2:5:2 , the flow rate is 1ml / min, the stati...

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Abstract

The invention relates to a fluoxertine hydrochloride compound and a new preparation method thereof. The method comprises the following steps of: step 1), dissolving a fluoxertine hydrochloride crude product into an organic solvent, and filtering and removing insoluble impurities to obtain primary filtrate; step 2), adding an adsorptive inorganic substance into the primary filtrate, vigorously stirring, standing still, filtering and removing the adsorptive inorganic substance to obtain secondary filtrate, and concentrating under the reduced pressure; step 3) using a preparation-type chromatographic column for separating and purifying the concentrated filtrate, and collecting eluent; step 4), heating up the eluent to not higher than 80 DEG C, maintaining for a period of time and concentrating, adding an adverse solvent while stirring, adding hydrochloric acid for adjusting the pH value to be within the range of 2.0-5.5, then, carrying out three-stage temperature reduction for recrystallization, and separating, washing and drying the separated crystal, thus obtaining the refined fluoxertine hydrochloride. The product prepared by the method is high in purity, and only one chromatographic peak is found to be available through high performance liquid chromatography. The method can be used for solving the problem of crude fluoxertine hydrochloride and fluoxertine hydrochloride bulk drug, has the characteristics of being simple, convenient, easy to control and easy in industrial production, and can be used for improving the preparation product quality and reducing the toxic and side effects.

Description

technical field [0001] The invention relates to a fluoxetine hydrochloride compound and a new preparation method for purifying it, belonging to the technical field of medicine. Background technique [0002] Fluoxetine Hydrochloride, white to off-white crystalline solid, melting point 158.4-158.9°C. Its chemical name is: (±)-N-methyl-γ-[4-(trifluoromethyl)-phenoxy]-amphetamine hydrochloride, molecular formula: C17H18F3NO·HCl, molecular weight: 345.11, and the structural formula is as follows [0003] [0004] At present, the traditional drugs for the treatment of depression are mainly tricyclic antidepressants, such as amitriptyline and clomipramine. The therapeutic effect of these drugs is definite, but a considerable number of patients have adverse reactions after taking the drugs, especially the high anticholinergic and cardiovascular system side effects, mainly manifested as dry mouth, constipation, headache, drowsiness, palpitations , tachycardia, and orthostatic sy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/48C07C213/10
Inventor 廖爱国
Owner HAINAN MEIDA PHARMA
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