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Preparation method for (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form I

A technology of pyrrolidine acetamide and -4-, which is applied in the field of preparation of -4-hydroxy-2-oxo-1-pyrrolidine acetamide crystal form, can solve the problems of disclosure, preparation method and crystal form research less, No questions about the crystal form of 4-hydroxy-2-oxo-1-pyrrolidineacetamide

Inactive Publication Date: 2018-05-01
CHONGQING RUNZE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently (R)-4-hydroxy-2-oxo-1-pyrrolidine acetamide preparation method and crystal form research is less, there is no (R)-4-hydroxy-2-oxo-1-pyrrolidine acetamide Amide crystal form disclosure

Method used

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  • Preparation method for (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form I
  • Preparation method for (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form I
  • Preparation method for (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 60 mg of (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide (Chongqing Runze Pharmaceutical Co., Ltd.) in 1 mL of methanol, heat at 50°C, and filter to obtain a supersaturated solution. Seal the solution and place it Cool and crystallize at -19°C for 24 hours, filter and separate, and dry at a temperature of 65°C and a relative humidity of 20% for about 6 hours to obtain crystals.

Embodiment 2

[0026] The (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal obtained in Example 1 was subjected to crystallographic determination.

[0027] Powder Diffraction Determination (XRPD):

[0028] Test instrument conditions: use Bruker D2PHASER powder diffractometer to test at room temperature, the test conditions are: Cu Ka It is the light source, the voltage is 30kV, the current is 10mA, the test step is 0.014°, the scanning speed is 0.1s / step, and the scanning range is 5-40° (2θ). After testing, the crystals of (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide prepared in Example 1 have diffraction angles 2θ of 12.6±0.2°, 14.04±0.2°, 15.1±0.2°, 16.66 ±0.2°, 17.54±0.2°, 19.42±0.2°, 20.68±0.2°, 21±0.2°, 22.16±0.2°, 23.46±0.2°, 25.36±0.2°, 26.08±0.2°, 26.5±0.2°, 30.26 There are diffraction peaks at ±0.2°, 30.46±0.2°, 30.96±0.2°, 31.28±0.2°. For convenience, this crystal is called "(R)-4-hydroxyl-2-oxo-1-pyrrolidine Acetamide crystal form I", its powder diffraction pattern is shown in ...

Embodiment 3

[0042] Dissolve 100mg of (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide in 2mL of methanol, heat at 45°C, and filter to obtain a supersaturated solution. Seal the solution and place it at -17°C for cooling Crystallization, separation by filtration, drying at 70°C and a relative humidity of 30% for about 7 hours to obtain colorless sand-like crystals, which were identified as (R)-4-hydroxy-2-oxo- 1-Pyrrolidineacetamide Form I.

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Abstract

The present invention provides a preparation method for an (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form. The method comprises the following steps: using methanol or butanone as a solvent, dissolving the (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide to prepare a supersaturated solution, performing crystallization at the low-temperature environment of -12 DEG C to -21 DEG C, performing filtration, and performing drying to obtain the (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form; and the crystal form has diffraction peaks at the diffraction angles of 16.66 + / - 0.2 degrees, 17.54+ / - 0.2 degrees, 21 + / - 0.2 degrees, 22.16 + / - 0.2 degrees and 30.96 + / - 0.2 degrees which are expressed in terms of 2theta. According to the present invention, the (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide crystal form prepared by the method has good flowability and is suitable for production of pharmaceutical preparations, storage and transportation; and after the crystal form is placed for 6months under simulated market packaging conditions, each detection index has no significant change and is in the specialized range, and the crystal form has good stability.

Description

technical field [0001] The present invention relates to (R)-4-hydroxyl-2-oxo-1-pyrrolidineacetamide, in particular to a preparation of (R)-4-hydroxyl-2-oxo-1-pyrrolidineacetamide crystal form method. Background technique [0002] 4-Hydroxy-2-oxo-1-pyrrolidineacetamide, CAS No. 62613-82-5, was first synthesized in 1974 by the Italian Skeleton Bichem Company, a new generation of brain metabolism-improving drug launched in 1987, It can promote the synthesis of phosphorylcholine and o-acethanolamine, promote brain metabolism, stimulate specific central nervous pathways through the blood-brain barrier, and improve intelligence and memory. Studies have shown (CN 106166150 A), (R)-4-hydroxy-2-oxo-1-pyrrolidineacetamide (CAS 68252-28-8), has special biological activity in the field of sedation and anti-epileptic, and It has low toxicity and wide range of drug safety, and is expected to become a substitute for the existing highly toxic antiepileptic drugs. For the effective develo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/273
CPCC07D207/273C07B2200/07C07B2200/13A61P25/08A61K31/4015
Inventor 叶雷
Owner CHONGQING RUNZE PHARM CO LTD
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