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Oxiracetam crystal form and preparation method thereof

A technology of crystal form and reflection angle, applied in the field of medicine, can solve the problems of purity and stability, unfavorable environmental protection and other problems, and achieve the effect of simple operation, good safety and cost reduction

Active Publication Date: 2013-10-09
CSPC OUYI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The Oxiracetam crystal form disclosed above, on the one hand, introduces a large amount of organic solvents in its preparation method, which is not conducive to environmental protection; on the other hand, there are also certain problems in purity and stability. The crystal form of racetam is very necessary

Method used

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  • Oxiracetam crystal form and preparation method thereof
  • Oxiracetam crystal form and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Preparation of Oxiracetam Crystal Form

[0048] a) Take 100 g of crude oxiracetam, add it to 200 ml of water, and heat to dissolve it to obtain an aqueous solution of oxiracetam;

[0049] b) Concentrate the above aqueous solution under reduced pressure to 50ml, the concentration temperature is 45-55°C, and the vacuum degree is -0.08MPa~-0.085MPa.

[0050] c) Cool the concentrated solution to 5°C, stir and crystallize for 1 hour, the stirring speed is 60 rpm, centrifuge to separate out the crystals, and then vacuum dry at a temperature of 45°C and a vacuum degree of -0.08MPa to -0.1MPa After 1 hour, 85.3 g of finished oxiracetam crystal form was obtained, the weight yield was 85.3%, the purity determined by HPLC was 99.89%, and the melting point was 168.2-170.0°C.

Embodiment 2

[0051] Example 2 Preparation of Oxiracetam Crystal Form

[0052] a) take 100 g of crude oxiracetam, add it into 600 ml of water, and dissolve it to obtain an aqueous solution of oxiracetam;

[0053] b) Add 5g of activated carbon to the above aqueous solution, stir and decolorize at 40-50°C for 0.5 hours, filter, and collect the filtrate;

[0054] c) Concentrate the above aqueous solution under reduced pressure to 300ml, the concentration temperature is 40-45°C, and the vacuum degree is -0.085MPa~-0.090MPa.

[0055] d) Cool the concentrated solution to 0°C, stir and crystallize for 6 hours, the stirring speed is 40 rev / min, separate the crystals by filtration, and then vacuum dry at a temperature of 55°C and a vacuum degree of -0.08MPa to -0.1MPa After 4 hours, 73.5 g of finished oxiracetam crystal form was obtained, the weight yield was 73.5%, the purity determined by HPLC was 99.95%, and the melting point was 168.1-169.5°C.

Embodiment 3

[0056] Example 3 Preparation of Oxiracetam Crystal Form

[0057] a) take 100 g of crude oxiracetam, add it into 1000 ml of water, and dissolve it to obtain an aqueous solution of oxiracetam;

[0058] b) Concentrate the above aqueous solution under reduced pressure to 200ml, the concentration temperature is 35-40°C, and the vacuum degree is -0.090MPa~-0.095MPa.

[0059] c) Cool the concentrated solution to 2°C, stir and crystallize for 3 hours, and the stirring speed is 30 r / min; separate the crystals by pressure filtration, and then vacuum at a temperature of 65°C and a vacuum degree of -0.08MPa~-0.1MPa After drying for 3 hours, 78.9 g of oxiracetam crystal form finished product was obtained, the weight yield was 78.9%, the purity measured by HPLC was 99.92%, and the melting point was 166.0-167.8°C.

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Abstract

The invention relates to an oxiracetam crystal form and a preparation method thereof. The oxiracetam crystal form is fewer in impurity and high in purity, especially is stable in crystal form, good in quality stability and excellent in particle fluidity, is beneficial to transportation, storage and production of pharmaceutical preparations and also can guarantee the curative effect and the safety of the pharmaceutical preparations in clinical application. The invention also provides the preparation method of the oxiracetam crystal form. The method is an environmentally-friendly process, only uses water as a solvent, and is simple to operate and low in production cost; and the prepared product has no residue of an organic solvent, is good in safety and is especially suitable for industrial production.

Description

technical field [0001] The invention relates to a medicinal crystal form and a preparation method thereof, in particular to a crystal form of oxiracetam and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Oxiracetam, the English name is Oxiracetam, the chemical name is 4-hydroxy-2-oxo-1-pyrrolidine acetamide, and the structural formula is shown in formula 1: [0003] [0004] Oxiracetam is a nootropic drug that can improve memory and learning in patients with senile dementia and memory impairment. The results of the study show that oxiracetam can promote the synthesis of phosphorylcholine and phosphorylethanolamine, and improve the brain The ratio of ATP / ADP increases the synthesis of proteins and nucleic acids in the brain. At present, it is widely used in clinic for the treatment of memory and intellectual impairment caused by mild to moderate vascular dementia, senile dementia and traumatic brain injury, with d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/273A61K31/4015A61P25/28
Inventor 李瑞建郑雪清杨英梅孙成勇郭倩张文静胡瑞娟陈丽
Owner CSPC OUYI PHARM CO LTD
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