Paroxetine hydrochloride compound and preparation method thereof

A technology for paroxetine hydrochloride and a compound, applied in the field of medicine, can solve problems such as low purity of paroxetine hydrochloride, and achieve the effects of easy industrial production, easy control, and improved product quality

Inactive Publication Date: 2013-03-06
HAINAN MEIDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the defects of the above-mentioned prior art, especially the low purity of paroxetine hydrochloride prepared by the prior art, the invention provides a method for preparing a high-purity paroxetine hydrochloride compound

Method used

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  • Paroxetine hydrochloride compound and preparation method thereof
  • Paroxetine hydrochloride compound and preparation method thereof
  • Paroxetine hydrochloride compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Accurately weigh 10 g of paroxetine hydrochloride raw material with a purity of 92.3% (Beijing Wansheng Pharmaceutical Co., Ltd., H20093150) and dissolve it in 50 ml of methanol, stir to make it completely dissolve, filter with suction, discard solid impurities, and collect the filtrate.

[0041] The methanol solution containing paroxetine hydrochloride is filled to a particle size of 75-165 μm and a pore size of A fine-pore silica gel column, then pumped into a mixed solvent of methanol and water with a volume ratio of 7:1 for elution, the column temperature is room temperature, and the flow rate is 1.2ml / min, and the elution site with a paroxetine hydrochloride content greater than 90% is collected. Concentrate under reduced pressure at 30°C at 0.1 MPa, and collect the concentrate.

[0042] Raise the methanol aqueous solution of paroxetine hydrochloride to 80°C, add 0.05M dilute hydrochloric acid aqueous solution accounting for 2 times its volume, adjust the pH value...

Embodiment 2

[0047] Accurately weigh 10 g of expired paroxetine hydrochloride raw material with a purity of 85.6% (Zhejiang Huahai Pharmaceutical Co., Ltd., H20031105) and dissolve it in 200 ml of methanol, stir to make it completely dissolve, filter with suction, discard solid impurities, and collect the filtrate.

[0048] The methanol solution containing paroxetine hydrochloride is filled to a particle size of 85-165 μm and a pore size of A fine-pore silica gel column, then pumped into a mixed solvent of methanol and water with a volume ratio of 6:1 for elution, the column temperature is room temperature, and the flow rate is 1.4ml / min, and the elution site where the paroxetine hydrochloride content is greater than 88% is collected, Concentrate under reduced pressure at 40°C at 0.08MPa, and collect the concentrate.

[0049] Raise the methanol aqueous solution of paroxetine hydrochloride to 75°C, add 0.01M dilute hydrochloric acid aqueous solution accounting for 1.5 times its volume, adj...

Embodiment 3

[0051] Accurately weigh 10 g of expired paroxetine hydrochloride raw material (Zhejiang Jianfeng Pharmaceutical Co., Ltd., H20040532) with a purity of 82.1% and dissolve it in 100 ml of methanol, stir to make it completely dissolve, filter with suction, discard solid impurities, and collect the filtrate.

[0052] The methanol solution containing paroxetine hydrochloride is filled to a particle size of 70-150 μm and a pore size of A fine-pore silica gel column, then pumped into a mixed solvent of methanol and water with a volume ratio of 5:1 for elution, the column temperature is room temperature, and the flow rate is 1.5ml / min, and the elution site where the paroxetine hydrochloride content is greater than 85% is collected, Concentrate under reduced pressure at 0.1MPa at 35°C, and collect the concentrate.

[0053] Raise the methanol aqueous solution of paroxetine hydrochloride to 70°C, add 0.008M dilute hydrochloric acid aqueous solution accounting for 3 times its volume, adj...

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Abstract

The invention relates to a paroxetine hydrochloride compound with the purity of larger 99.5% and the following structural formula, and also relates to a preparation of the paroxetine hydrochloride compound. The preparation method comprises the following steps of: (1) dissolving the raw material paroxetine hydrochloride in the proper amount of methanol, extrating and filtering, abandoning solid impurities, and obtaining a methanol solution containing the paroxetine hydrochloride; (2) carrying out column chromatography on the methanol solution containing the paroxetine hydrochloride to load samples, collecting paroxetine hydrochloride elution parts, decompressing, concentrating, and obtaining a paroxetine hydrochloride methanol solution; and (3) adding an aqueous solution of diluted hydrochloric acid of 0.001-0.1M to the paroxetine hydrochloride methanol solution at the temperature not higher than 80 DEG C, regulating a pH value to be 4-6, reducing temperature in a gradient manner, re-crystallizing, and obtaining the purified paroxetine hydrochloride compound. The paroxetine hydrochloride compound disclosed by the invention has higher purity, the production quality of preparation is improved, the toxic and side effects are reduced, and the preparation method is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a high-purity paroxetine hydrochloride compound and a preparation method, belonging to the technical field of medicine. Background technique [0002] Paroxetine Hydrochloride (Paroxetine Hydrochloride), the chemical name is (3s) trans-3-[(1,3-benzodioxol-5-yloxy(yl))methyl]-4-(4-fluorobenzene Base) piperidine hydrochloride, molecular formula C 19 h 20 FNO 3 ·HCl·1 / 2H 2 O, structural formula: [0003] [0004] Paroxetine hydroehloride is a powerful and highly effective selective central nervous system 5-HT reuptake inhibitor. It inhibits the active transport of 5-HT, increases the concentration of 5-HT in the synaptic space, and strengthens the nerve conduction of 5-HT to play an antidepressant effect. , had minimal effects on norepinephrine and dopamine reuptake. It and toxin receptors, α-adrenergic receptors, β-adrenoceptors, dopamine D 2 receptor, histamine H 1 receptor, 5-HT 2 The receptor has almost no affinity,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/12
Inventor 廖爱国
Owner HAINAN MEIDA PHARMA
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