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A kind of donepezil hydrochloride crystal form compound and preparation method thereof

A technology of donepezil hydrochloride and its compound, which is applied in the field of medicine, can solve problems such as poor drug stability, and achieve the effects of good stability, high dissolution rate and bioavailability, and simple preparation method

Active Publication Date: 2019-03-08
SHANDONG LUOXIN PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the above-mentioned problems in the prior art, the present invention provides a new crystal form of donepezil hydrochloride, which has good stability, solves the defect of poor drug stability in the application process of donepezil hydrochloride in the prior art, and provides a new crystal form resources

Method used

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  • A kind of donepezil hydrochloride crystal form compound and preparation method thereof
  • A kind of donepezil hydrochloride crystal form compound and preparation method thereof
  • A kind of donepezil hydrochloride crystal form compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Take 15 g of donepezil hydrochloride in a reaction flask, add 300 ml of a mixed solution of dimethyl sulfoxide and ethanol (the volume ratio of dimethyl sulfoxide and ethanol is 5:1), heat to 40 ° C, stir to dissolve, and filter while hot ;While stirring, the temperature was lowered to 20°C (the cooling rate was 5°C per minute), and the pre-cooled mixed solvent B was added to the solution at a flow rate of 1.0mL / min (the volume ratio of ethanol and dichloromethane was 1:3) 600ml until the crystals appear, continue to cool down to -5°C (the cooling rate is 1°C per minute), and stir for 3h. After vacuum filtration, the filter cake was vacuum-dried at 50° C. for 6 h to obtain 13.0 g of white needle-like solid, with a yield of 86.3%.

[0029] Related analysis tests:

[0030] 1. X-ray powder diffraction test:

[0031] Instrument model: BrukerD8ADVANCE; light source Cu-Ka40kV40mA; graphite monochromator; divergence slit (DS): 1°; LynxEye array detector, scanning mode: θ / θ, ...

Embodiment 2

[0036] Take 10 g of donepezil hydrochloride in a reaction flask, add 100 ml of a mixed solution of dimethyl sulfoxide and ethanol (the volume ratio of dimethyl sulfoxide and ethanol is 6:1), heat to 50 ° C, stir to dissolve, and filter while hot ;While stirring, the temperature was lowered to 25°C (the cooling rate was 5°C per minute), and the pre-cooled mixed solvent B was added to the solution at a flow rate of 1.5mL / min (the volume ratio of ethanol and dichloromethane was 1:3) 300ml until the crystals appear, continue to cool down to -10°C (the cooling rate is 1°C per minute), and stir for 2h. After vacuum filtration, the filter cake was vacuum-dried at 50° C. for 4 hours to obtain 9.06 g of white needle-like solid, with a yield of 90.6%. The X-ray powder diffraction spectrum of the obtained crystal measured by Cu-Kα rays is similar to that of Example 1.

Embodiment 3

[0038] Take 15g of donepezil hydrochloride in a reaction flask, add 225ml of a mixed solution of dimethyl sulfoxide and ethanol (the volume ratio of dimethyl sulfoxide and ethanol is 4:1), heat to 45°C, stir to dissolve, and filter while hot ;While stirring, the temperature is lowered to 30°C (the cooling range is 5°C per minute), and 1125ml of pre-cooled mixed solvent B (the volume ratio of ethanol and dichloromethane is 1:3) is added to the solution at a flow rate of 2mL / min Until the crystals appear, continue to cool down to -5°C (the cooling rate is 1°C per minute), and stir for 2h. After vacuum filtration, the filter cake was vacuum-dried at 50° C. for 5 h to obtain 13.7 g of white needle-like solid, with a yield of 91.5%. The X-ray powder diffraction spectrum obtained by measuring the prepared donepezil hydrochloride crystals using Cu-Kα rays is similar to that of Example 1.

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Abstract

The invention discloses a donepezil hydrochloride crystal form compound and a preparation method thereof. An X-ray powder diffraction pattern obtained by using Cu-Kalpha ray is represented by figure 1. The donepezil hydrochloride crystal form compound has the advantages of simple crystal form, high purity, good stability, high solubility, high dissolubility and high bioavailability. The crystal form has high stability, keeps stable even under strict strong conditions, and does not change in the subsequent preparation or storage process of preparations. The production method has the advantages of simplicity, low cost, and easy realization of large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a crystal form of donepezil hydrochloride and a preparation method thereof. Background technique [0002] Donepezil Hydrochloride (DH), Chinese chemical name is 1-benzyl-4-[(5,6-dimethoxy-1-indanone)-2-methylene]piperidine hydrochloride, molecular formula for C 24 h 29 NO 3 HCl, molecular weight is 415.96, CAS number is 120011-70-3, the molecular structure formula of donepezil hydrochloride is as follows: [0003] [0004] Donepezil hydrochloride is a second-generation cholinesterase (CHE) inhibitor, a long-acting symptomatic drug for Alzheimer's disease, and the only drug approved by the US FDA and the British Ministry of Health Medicines Administration (MCA) at the same time Compared with similar drugs, donepezil hydrochloride has the characteristics of long action time, high efficacy, high safety, and small adverse drug reactions. At present, it has been listed in m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/32
CPCC07B2200/13C07D211/32
Inventor 宋丽丽朱传喜刘广俄
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
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