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Preparation method for flunarizine hydrochloride crystal

A crystallization technology of flunarizine hydrochloride, which is applied in the field of preparation of crystallization of flunarizine hydrochloride to achieve the effects of complete crystal form, low labor intensity and uniform particle size distribution

Active Publication Date: 2019-11-19
迪嘉药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no literature reports on how to prepare flunarizine hydrochloride bulk drug products with stable performance and good fluidity through crystallization, and the powder properties of flunarizine hydrochloride bulk drugs (such as particle size distribution, fluidity, etc.) Regulation is still a blank area

Method used

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  • Preparation method for flunarizine hydrochloride crystal
  • Preparation method for flunarizine hydrochloride crystal
  • Preparation method for flunarizine hydrochloride crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 20 g of flunarizine hydrochloride into a three-necked flask filled with 200 mL of a mixed solvent of methanol and water (the volume ratio of methanol to water is 90:10), raise the temperature to 50°C and stir to dissolve. Then add activated carbon for decolorization and filter; transfer the filtrate to a crystallizer at 50°C, start to evaporate and crystallize, control the vacuum degree of the system at 0.03MPa, and the evaporation rate is 30mL / hour. After growing the crystal for 30 minutes, continue to evaporate and crystallize, and stop the evaporation when the total amount of solvent evaporated reaches 60 mL. The crystal was grown with heat preservation and stirring for 30 minutes, and then the temperature was lowered to 5° C. with stirring at a cooling rate of 5° C. / hour, and the temperature was kept and stirred for 1 hour. Suction filtration, and rinse the filter cake with methanol, and dry at 40°C under normal pressure for 8 hours to obtain 18.06g block-shaped...

Embodiment 2

[0031] Add 20g of flunarizine hydrochloride into a three-necked flask filled with 300mL of ethanol and water mixed solvent (the volume ratio of ethanol to water is 95:5), raise the temperature to 65°C and stir to dissolve. Then add activated carbon for decolorization and filter; transfer the filtrate to a crystallizer at 65°C, start to evaporate and crystallize, control the vacuum degree of the system at 0.05MPa, and the evaporation rate is 50mL / hour. After growing the crystal for 45 minutes, continue to evaporate and crystallize, and stop evaporation when the total amount of solvent evaporated reaches 195 mL. The crystal was grown with heat preservation and stirring for 120 minutes, and then the temperature was lowered to 8° C. with stirring at a cooling rate of 6° C. / hour, and the heat preservation and stirring were carried out for 45 minutes. Suction filtration, rinse the filter cake with ethanol, and dry under normal pressure at 60°C for 10 hours to obtain 18.27g of block-...

Embodiment 3

[0033] Add 20g of flunarizine hydrochloride into a three-necked flask filled with 400mL of ethanol and water mixed solvent (the volume ratio of ethanol to water is 85:15), raise the temperature to 50°C and stir to dissolve. Then add activated carbon to decolorize and filter; transfer the filtrate to a crystallizer at 65°C, start to evaporate and crystallize, control the vacuum degree of the system at 0.04MPa, and the evaporation rate is 60mL / hour. After growing the crystal for 45 minutes, continue to evaporate and crystallize, and stop evaporation when the total amount of solvent evaporated reaches 200mL. The crystal was grown with heat preservation and stirring for 100 minutes, and then the temperature was lowered to 5° C. with stirring at a cooling rate of 5° C. / hour, and the heat preservation and stirring were carried out for 45 minutes. Suction filtration, rinse the filter cake with ethanol, and dry under normal pressure at 60°C for 12 hours to obtain 18.06 g of block-shap...

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Abstract

The invention relates to a preparation method for a flunarizine hydrochloride crystal. The invention relates to a preparation method for a flunarizine hydrochloride crystal with a particle size of 20-30 microns. The preparation method comprises the following steps: firstly, adding flunarizine hydrochloride into an aqueous solution of a low-boiling-point organic solvent; carrying out reduced-pressure evaporation at a temperature of 50-80 DEG C and a vacuum degree of 0.03-0.08 MPa, evaporating out a part of the solvent at an evaporation rate of 10-25% / h of the total amount of the solvent, performing crystal growing for 30-60 min after the crystal is separated out, then continuously carrying out reduced-pressure evaporation, and stopping evaporation and performing crystal growing when the volume of a distillate is 30-65% of the volume of the solvent; carrying out cooling to 5-10 DEG C at a cooling speed of 5-10 DEG C / h, and maintaining the temperature for crystal growing for 30-60 min; and carrying out filtering, and washing a filter cake with a solvent. The invention provides the preparation method for the flucinarizine hydrochloride crystal with controllable granularity.

Description

technical field [0001] The invention relates to a preparation method of flunarizine hydrochloride crystals, belonging to the technical field of crystallization. Background technique [0002] With the continuous advancement of technology in the pharmaceutical industry, more and more studies have found that the powder quality index of drugs is one of the key factors affecting the development and quality control of oral solid dosage forms. Particle size and its distribution, as an important indicator of drug powder properties, will not only affect the appearance of the drug, but also directly affect the production efficiency of filtration, washing, drying and other processes, and will also affect the dissolution rate and content uniformity of the drug. , stability and other indicators have a considerable impact. [0003] Flunarizine Hydrochloride (Flunarizine Hydrochloride), chemical name (E)-1-[bis-(4-fluorophenyl)methyl]-4-(2-propenyl-3-phenyl)piperazine disalt Salt, mole...

Claims

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Application Information

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IPC IPC(8): C07D295/073
CPCC07D295/073
Inventor 王冠姜凯姚岩孙详彧刘世超王超
Owner 迪嘉药业集团股份有限公司
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