Crystal form B of flunarizine hydrochloride and preparation method thereof

A technology of flunarizine hydrochloride and its crystal form, which is applied in the field of flunarizine hydrochloride crystal form B and its preparation, can solve problems not involved in polymorph research, etc., and achieve favorable storage, simple preparation method, and hygroscopicity Reduced effect

Active Publication Date: 2020-01-21
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

[0010] For flunarizine hydrochloride, most of the published literature currently reports its synthesis method and optimization, and does not involve its polymorphic research

Method used

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  • Crystal form B of flunarizine hydrochloride and preparation method thereof
  • Crystal form B of flunarizine hydrochloride and preparation method thereof
  • Crystal form B of flunarizine hydrochloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 10 g of flunarizine hydrochloride into 330 g of acetonitrile aqueous solution (mass ratio, acetonitrile: water = 4:1), stir continuously at 65°C for about 40 min until dissolved; add activated carbon, stir for 40 min to decolorize, and filter with suction ; Move the filtrate into a crystallizer at 50°C and keep it warm; add 330 g of acetonitrile to the crystallizer at a constant speed within 1 hour, and continue to stir at a constant temperature for 2 hours after the overall solution is obviously turbid; then slowly cool the system down to 35°C within 3 hours , and stirred at a constant temperature for 4 h at the end of cooling; then quickly cooled the system to 10°C within 30 min, and stirred at a constant temperature for 1 h at the end of cooling; filtered with suction, washed the filter cake with 70% acetonitrile aqueous solution; collected the filter cake, and dried it at 65°C Vacuum (0.08MPa) dried for 12 h, collected the product, and obtained 8.56 g of white gr...

Embodiment 2

[0038]Put 10 g of flunarizine hydrochloride into 100 g of acetonitrile aqueous solution (mass ratio, acetonitrile: water = 7:3), stir continuously at 70°C for about 1 h until dissolved; add activated carbon, stir for decolorization for 60 min, and filter with suction ; Move the filtrate into a crystallizer at 55°C and keep it warm; add 300 g of acetonitrile to the crystallizer at a constant speed within 30 min, and continue to stir at a constant temperature for 1 h after the overall solution is obviously turbid; then slowly cool the system down to 45°C within 4 h. ℃, and stirred at a constant temperature for 2 h at the end of cooling; then quickly cooled the system to 5 °C within 45 min, and stirred at a constant temperature for 3 h at the end of cooling; filtered with suction, and washed the filter cake with 80% acetonitrile aqueous solution; The product was dried under vacuum (0.1MPa) for 15 h, and the product was collected to obtain 9.23 g of white granular flunarizine hydro...

Embodiment 3

[0040] Put 10 g of flunarizine hydrochloride into 180 g of acetonitrile aqueous solution (mass ratio, acetonitrile: water = 3:1), stir continuously at 65°C for about 40 min until dissolved; add activated carbon, stir for 50 min to decolorize, and filter with suction ; Move the filtrate into a crystallizer at 52°C and keep it warm; add 270 g of acetonitrile to the crystallizer at a uniform speed within 45 minutes, and continue to stir at a constant temperature for 90 minutes after the overall solution is obviously turbid; then slowly cool the system to 40 within 2 hours. ℃, and stirred at a constant temperature for 2 h at the end of cooling; then quickly cooled the system to 6°C within 40 min, and stirred at a constant temperature for 30 min at the end of cooling; filtered with suction, and washed the filter cake with 75% acetonitrile aqueous solution; The product was dried under vacuum (0.08 MPa) for 15 h, and the product was collected to obtain 8.69 g of white granular flunari...

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Abstract

The invention relates to a novel crystal form of flunarizine hydrochloride and a preparation method thereof, and belongs to the technical field of medicine crystallization. According to a technical scheme, the X-ray powder diffraction pattern of the crystal form B of the flunarizine hydrochloride has the following characteristic peaks at 2[theta]+ / -0.2 degrees: 6.35, 6.55, 8.76, 12.76, 13.07, 13.83, 14.17, 14.36, 14.67, 14.93, 15.60, 15.78, 16.64, 17.18, 17.56, 18.19, 18.45, 18.90, 19.05, 19.65 and 19.84. The invention provides the novel crystal form with stable performance of the flunarizinehydrochloride and a preparation method thereof.

Description

technical field [0001] The invention relates to flunarizine hydrochloride crystal form B and a preparation method thereof, belonging to the technical field of medicine crystallization. Background technique [0002] Flunarizine Hydrochloride (Flunarizine Hydrochloride) is a diphenylpiperazine developed by Belgian Janssen Company for the treatment of cerebral blood supply insufficiency, vertebral artery ischemia, cerebral thrombosis, tinnitus, dizziness, migraine and epilepsy. derivative. The drug was first launched in some European countries in the early 1980s, and in 1989 in my country. Flunarizine hydrochloride is white or off-white crystal or crystalline powder; odorless and tasteless. Its chemical name is: (E)-1-[bis(4-fluorophenyl)methyl]-4-(2-propenyl-3-phenyl)-piperazine dihydrochloride, and its chemical structure is as follows Show. [0003] [0004] Flunarizine hydrochloride is slightly soluble in methanol or ethanol, slightly soluble in chloroform, very sligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/073
CPCC07D295/073C07B2200/13
Inventor 王冠孙详彧姜凯姚岩王超徐西坤
Owner 迪嘉药业集团股份有限公司
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