A kind of flucloxacillin sodium crystal form, preparation method and application

The technology of flucloxacillin sodium crystal and flucloxacillin sodium is applied in the field of medicine, can solve problems such as enlargement, and achieves the effects of simple preparation method, controlled production cost and easy drying

Active Publication Date: 2018-01-16
GUILIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product is dried at high temperature for a long time, which poses a great challenge to the quality of the product, because the drying time is too long, and the risk of impurities in the product increases at high temperature

Method used

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  • A kind of flucloxacillin sodium crystal form, preparation method and application
  • A kind of flucloxacillin sodium crystal form, preparation method and application
  • A kind of flucloxacillin sodium crystal form, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Get 50g flucloxacillin sodium, dissolve in 250g acetone, filter to obtain solution A, control the temperature of solution A at 0°C;

[0038] (2) Take 180g of isopropyl ether, add it to the solution A obtained in step (1), stir for 30min, and cool down to -5°C to obtain solution B;

[0039] (3) Take 100g of methyl acetate and add it to the solution B obtained in step (2) within 3 hours. After the dropwise addition, stir and crystallize for 2 hours. After filtering, dry it under reduced pressure at 50°C at -0.08~-0.09MPa , to obtain the new crystal form of flucloxacillin sodium.

[0040] Depend on figure 1 As shown in the infrared spectrum, at 792cm -1 、896cm -1 、1249cm -1 、1323cm -1 、 1400cm -1 、1454cm -1 、1508cm -1 、1600cm -1 、1770cm -1 、2977cm -1 and 3367cm -1 Has characteristic absorption.

[0041] Among them, at 1454cm -1 、1508cm -1 and 1600cm -1 There is vibration of the benzene ring skeleton, 792cm -1 Three adjacent = C-H out-of-plane bending v...

Embodiment 2

[0048] (1) Get 50g flucloxacillin sodium, dissolve in 350g acetone, filter to obtain solution A, control the temperature of solution A at 9°C;

[0049] (2) Take 130g of isopropyl ether, add it to the solution A obtained in step (1), stir for 30min, and cool down to -10°C to obtain solution B;

[0050] (3) Take 170g of methyl acetate and add it to the solution B obtained in step (2) within 4 hours. After the dropwise addition, stir and crystallize for 2 hours. After filtering, dry under reduced pressure at 60°C at -0.08~-0.09MPa , to obtain the new crystal form of flucloxacillin sodium.

Embodiment 3

[0052] (1) Get 50g flucloxacillin sodium, dissolve in 350g acetone, filter to obtain solution A, control the temperature of solution A at 15°C;

[0053] (2) Take 100 g of isopropyl ether, add it to the solution A obtained in step (1), stir for 30 minutes, and cool down to -10°C to obtain solution B;

[0054] (3) Take 120g of ethyl acetate and add it to the solution B obtained in step (2) within 3.5h. After the dropwise addition, stir and crystallize for 2h. After filtering, dry under reduced pressure at 45°C at -0.08~0.09MPa , to obtain the new crystal form of flucloxacillin sodium.

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Abstract

The invention discloses a new flucloxacillin sodium crystal form as well as a preparation method and an application thereof, and belongs to the field of medical technologies. An X-ray powder diffraction pattern of the new flucloxacillin sodium crystal form has a strongest diffraction peak namely I / I0=100 when 2theta=11.377 degrees; and an infrared spectrum has characteristic absorption at 792, 896, 1249, 1323, 1400, 1454, 1508, 1600, 1770, 2977 and 3367 cm<-1>. The preparation method comprises the following steps: dissolving flucloxacillin sodium into a ketone solvent, and filtering to obtain a solution A; adding an ether solvent into the solution A, stirring, and cooling to obtain a solution B; and adding an ester solvent into the solution B, stirring for crystallization, filtering, and performing vacuum drying to obtain the new crystal form. The invention also discloses the application of the new crystal form. The new crystal form is easy to dry, can effectively reduce the drying time and reduce the risk of impurity increase, and has a relatively good effect for quality control.

Description

technical field [0001] The invention relates to a new crystal form of flucloxacillin sodium, a preparation method and application thereof, and belongs to the technical field of medicine. Background technique [0002] When a substance is crystallized, due to the influence of various factors, the intramolecular or intermolecular bonding mode changes, so the molecules or atoms are arranged differently in the lattice space to form different crystal structures. That is, the same substance has two or more spatial arrangements and unit cell parameters, and the phenomenon of forming multiple crystal forms is called polymorphism. When the substance is dissolved or melted, the lattice structure is destroyed, and the polymorphism disappears. [0003] Drug polymorphism widely exists in the production and research of solid drugs, and it is one of the main reasons affecting the efficacy of solid drugs. Appropriate and uniform crystal form is conducive to improving the efficacy of the dr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D499/76C07D499/18A61K31/431A61P31/04
CPCA61K31/431C07B2200/13C07D499/18C07D499/76
Inventor 苏钦璐潘梅彭斌林梅芳覃坚和
Owner GUILIN PHARMA
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