New crystal form of methylprednisolone aceponate and preparation method

A kind of technology of methylprednisolone acetonide and crystal, applied in the new crystal form of methylprednisolone acetonide and the field of preparation thereof, can solve the problems such as no report on the crystal form of methylprednisolone acetonide

Inactive Publication Date: 2012-09-12
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, there is no other related crystal form report of methylprednisolone acetate

Method used

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  • New crystal form of methylprednisolone aceponate and preparation method
  • New crystal form of methylprednisolone aceponate and preparation method
  • New crystal form of methylprednisolone aceponate and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Get 1kg of methylprednisolone acetate and completely dissolve it in 10L of tetrahydrofuran, then add a dissolution agent mixed with 5L of water and 5L of ethanol to the tetrahydrofuran in which methylprednisolone acetate has been dissolved, add it slowly while adding the dissolution agent While oscillating, until the turbidity that appeared when the eluent was just added disappears, evaporate under reduced pressure after the addition, and cool down, filter, and dry after crystals appear. The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate. X-ray powder diffraction measurement, the measured characteristic peak positions are 2θ=8.6°, 12.2°, 13.6°, 15.3°, 19.3°, such as figure 2 shown.

Embodiment 2

[0028] Get 1kg of methylprednisolone acetate and dissolve it completely in 40L of acetonitrile, then add 4L of water and 20L of normal hexane as a dissolution agent to the acetonitrile in which methylprednisolone acetate has been dissolved, add slowly while adding the dissolution agent While oscillating, until the turbidity that appeared when the eluent was just added disappears, evaporate under reduced pressure after the addition, and cool down, filter, and dry after crystals appear. The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate. X-ray powder diffraction measurement, the measured characteristic peak positions are 2θ=8.6°, 12.2°, 13.6°, 15.3°, 19.3°.

Embodiment 3

[0030] Add 0.2 g of methylprednisolone acetate into a mixed solution of 6 mL of tetrahydrofuran, 1 mL of water, and 2 mL of methanol, and stir until completely dissolved. The solution was transferred to a small beaker, sealed with parafilm, and a few small holes were punched on the film to facilitate solvent evaporation. After standing at room temperature for several days, crystallization was obtained. The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate. X-ray powder diffraction measurement, the measured characteristic peak positions are 2θ=8.5°, 12.1°, 13.6°, 15.3°, 19.3°, such as image 3 shown.

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Abstract

The invention relates to a new crystal form of methylprednisolone aceponate and a preparation method. According to the new crystal form, X-ray powder diffraction has characteristic peaks at diffraction angles 2 theta of 8.6 degrees, 12.2 degrees, 13.6 degrees, 15.3 degrees, 18.6 degrees and 19.3 degrees. According to the method, the methylprednisolone aceponate is dissolved in a mixed solution of water and an organic solvent completely, and the organic solvent is evaporated so as to prepare a methylprednisolone aceponate crystal.

Description

[0001] This application is the application number 201010150387.0, the filing date is April 20, 2010, and the divisional application of the Chinese patent application titled "A new crystal form of methylprednisolone acetate and its preparation method". Technical field: [0002] The invention relates to a steroid compound, in particular to a new crystal form of methylprednisolone acetate and a preparation method thereof. Background technique: [0003] The chemical structural formula of methylprednisolone acetate (Methylprednisolone aceponate, MPA, CAS: 86401-95-8) is as follows: [0004] [0005] Methylprednisolone acetate is developed by Schring AG of Germany as a derivative of methylprednisolone. It is a glucocorticoid with strong local anti-inflammatory activity and is used for the treatment of skin inflammation. At present, commercially available Methylprednisolone acetidine skin preparations are produced by Schring AG in Germany, and the trade name is Advantan 0.1% met...

Claims

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Application Information

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IPC IPC(8): C07J5/00
Inventor 何运良李静
Owner TIANJIN JINYAO GRP
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