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One step preparation method of paluxitin hydrochloride A crystal type crystal molecule assembly

A technology of paroxetine hydrochloride and crystals, which is applied in the field of one-step preparation of paroxetine hydrochloride A crystal crystal molecular assembly, which can solve the problems of increasing operation difficulty, affecting the quality of final products, and long operation time

Active Publication Date: 2005-08-10
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Invention CN1143643A has the following problems: 1) the steps are cumbersome, and to prepare paroxetine hydrochloride A crystal form crystals, paroxetine hydrochloride solvate must first be prepared, and then a qualified product can be obtained through the desolvation process of paroxetine hydrochloride solvate; 2) hydrochloric acid The desolvation process of the paroxetine solvate compound is also difficult to implement, and practice has proved that the desolvation process of the above-mentioned cases in this invention all obtains a mixture of anhydrous and paroxetine hydrochloride hemihydrate; 3) paroxetine hydrochloride in the above-mentioned cases in this invention Form A crystal preparation process, harsh conditions, long operation time, and low batch processing repeatability; 4) The final product obtained in the above case in this invention has too high solvent residue (about 4-14%); inventions WO00 / 32591, WO00 The problems in / 32592 and WO00 / 32595 are 1) the participation of ultrasonic waves will inevitably increase the difficulty of operation and increase the product cost; 2) the addition of additives in the crystallization process will definitely affect the quality of the final product

Method used

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  • One step preparation method of paluxitin hydrochloride A crystal type crystal molecule assembly
  • One step preparation method of paluxitin hydrochloride A crystal type crystal molecule assembly
  • One step preparation method of paluxitin hydrochloride A crystal type crystal molecule assembly

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] A crystalline form of paroxetine hydrochloride was prepared by using a mixture of ketones and alcohols as a solvent.

[0027] Add 20.0012g of paroxetine hydrochloride hemihydrate into a jacketed 500ml glass crystallizer, add 300ml of acetone and 60ml of isopropanol at the same time, stir together, and heat to 55°C, stirring continuously for 40 minutes, paroxetine hydrochloride hemihydrate is completely dissolved .

[0028] The air is naturally cooled, and crystals are precipitated at about 30°C. Continue to stir, and the crystallizer is obviously turbid in about 3 minutes, and continue to stir for 2 hours.

[0029] After suction filtration for 15 minutes, the filter cake was dried under high vacuum with phosphorus pentoxide for 2 hours at a drying temperature of 50°C.

[0030] 14.6556 g of anhydrous paroxetine hydrochloride was obtained, with acetone content of 0.26% (NMR analysis), isopropanol content of 0.10% (NMR analysis), and water content of 0.32% (KF).

[0031]...

example 2

[0039] A crystalline form of paroxetine hydrochloride was prepared by using fatty alcohol as a solvent.

[0040] Add 10.0235g of paroxetine hydrochloride hemihydrate in a 700ml jacketed crystallizer, add 500ml of ethanol at the same time, stir together, and heat to 55°C, continue stirring for 60 minutes, paroxetine hydrochloride hemihydrate is completely dissolved.

[0041] The air is naturally cooled, and crystals are precipitated at about 35°C, and the crystallizer is obviously turbid in about 3 minutes, and the stirring is continued for 1 hour.

[0042] After suction filtration for 20 minutes, the filter cake was dried under high vacuum with phosphorus pentoxide for 1 hour at a drying temperature of 45°C.

[0043] 8.6532 g of paroxetine hydrochloride in crystal form A was obtained, with an ethanol content of 0.35% (NMR analysis) and a water content of 0.26% (KF).

[0044] The melting point is 122-124°C.

[0045] The DSC test results with a heating rate of 10K / min show tha...

example 3

[0052] Using ketones as solvents, the A crystal form of paroxetine hydrochloride was prepared.

[0053] Add 8.8235g of paroxetine hydrochloride hemihydrate in a 700ml jacketed crystallizer, add 500ml of acetone at the same time, stir together, and heat to 50°C, continue stirring for 60 minutes, paroxetine hydrochloride hemihydrate is completely dissolved.

[0054] The air is naturally cooled, and crystals are precipitated at about 30°C, and the crystallizer is obviously turbid in about 3 minutes, and the stirring is continued for 3 hours.

[0055] Suction filtration was performed for 30 minutes, and the filter cake was dried under high vacuum with phosphorus pentoxide for 3 hours at a drying temperature of 55°C.

[0056] 7.1532 g of anhydrous paroxetine hydrochloride was obtained, with an acetone content of 0.35% (NMR analysis) and a water content of 0.25% (KF).

[0057] The melting point is 122-124°C.

[0058] The DSC test results with a heating rate of 10K / min show that th...

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Abstract

A process for preparing paroxetine A hydrochloride includes such steps as adding semi-hydrous paroxetine hydrochloride and solvent (oxylipohydrocarbon derivative) to the crystallizer with jacket, heating, stirring, natural cooling while educting out crystal, and stirring for 30-120 min.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to a one-step preparation method for paroxetine hydrochloride A crystal molecule assembly. technical background [0002] Paroxetine Hydrochloride, the full name is (3S,4R)-3-(3',4'-dioxymethylenephenoxymethyl)-4-(4'-fluorophenyl)piperidine hydrochloride. [(3S,4R)-3-(3',4'-methylenedioxyphenoxymethyl)-4-(4'-fluorophenyl)piperidine], the chemical formula is C 19 h 21 ClFNO 3 , the structural formula is as figure 1 shown. Paroxetine hydrochloride usually exists in the form of the hemihydrate. Paroxetine hydrochloride hemihydrate is white or near-white crystalline powder; its molecular weight is 374.8, and its theoretical water content is 2.4%. It is slightly soluble in water, easily soluble in methanol, almost insoluble in ethanol and dichloromethane; melting point is 128-132°C. [0003] Paroxetine Hydrochloride is a selective 5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/12
Inventor 王静康周明华张美景尹秋响任国宾
Owner TIANJIN UNIV
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