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Methylprednisolone aceponate monohydrate, crystal form and preparation method thereof

A technology of methylprednisolone acetate and monohydrate, which is applied in the field of new crystal forms of methylprednisolone acetate and its preparation, and can solve problems such as no reports of crystal forms of methylprednisolone acetate

Active Publication Date: 2010-06-30
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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  • Methylprednisolone aceponate monohydrate, crystal form and preparation method thereof
  • Methylprednisolone aceponate monohydrate, crystal form and preparation method thereof
  • Methylprednisolone aceponate monohydrate, crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Get 1g of methylprednisolone acetidine and dissolve it completely in 10mLTHF, then add a dissolving agent mixed by 5mL water and 5mL ethanol to the THF that has dissolved methylprednisolone acetate, slowly add when adding the dissolving agent, add while adding Vibrate until the turbidity that appeared when the eluent was just added disappears. After the addition, evaporate under reduced pressure. After the crystals appear, cool down, filter, and dry. The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate.

[0027] Molecular formula: C 27 h 38 o 8

[0028] Theoretical value of elemental analysis: C, 66.10; H, 7.81; O, 26.09

[0029] Elemental analysis found values: C, 65.98; H, 7.86; O, 26.16

[0030] And the obtained crystal is subjected to crystal parameter determination a=12.595 b=14.515 c=14.591 α90.00, β90.00, γ90.00, the unit cell volume is 2667.5 The crystal bel...

Embodiment 2

[0033] Get 0.5g methylprednisolone acetate and dissolve completely in 20mL acetonitrile, then add 2mL water and 10mL n-hexane as dissolution agent respectively in the acetonitrile that has dissolved methylprednisolone acetate, slowly add when adding dissolution agent, while While adding, vibrate until the turbidity that appeared when the eluent was just added disappears. After the addition, evaporate under reduced pressure. After the crystals appear, cool down, filter, and dry. The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate.

[0034] Molecular formula: C 27 h 38 o 8

[0035] Theoretical value of elemental analysis: C, 66.10; H, 7.81; O, 26.09

[0036] Elemental analysis found values: C, 65.96; H, 7.87; O, 26.17

[0037] And the obtained crystal is subjected to crystal parameter determination a=12.595 b=14.515 c=14.591 α90.00, β90.00, γ90.00, the unit cell volume is 266...

Embodiment 3

[0040]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. Single crystals were obtained after standing at room temperature for several days. . The water content of the dried crystal was measured by the Karl Fischer method, and it was confirmed to be methylprednisolone acetate monohydrate.

[0041] Molecular formula: C 27 h 38 o 8

[0042] Theoretical value of elemental analysis: C, 66.10; H, 7.81; O, 26.09

[0043] Elemental analysis found values: C, 66.01; H, 7.79; O, 26.20

[0044] And the obtained crystal is subjected to crystal parameter determination a=12.595 b=14.515 c=14.591 α90.00, β90.00, γ90.00, the unit cell volume is 2667.5 The crystal belongs to the orthorhombic crystal system, space group,...

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Abstract

The invention provides a methylprednisolone aceponate monohydrate, a crystal form and a preparation method thereof. The crystal parameters of the methylprednisolone aceponate monohydrate are alpha 90.00, beta 90.00, gamma 90.00, crystal cell volume is that the crystal belongs to a rhombic system, and the space group is P212121. X-ray powder diffraction is used for measurement, the X-ray powder diffraction of the methylprednisolone aceponate monohydrate has characteristic peaks when the diffraction angle 2theta is equal to 8.6 degrees, 12.2 degrees, 13.6 degrees, 15.3 degrees, 18.6 degrees, 19.3 degrees and 20.5 degrees, and the relative diffraction intensity of the methylprednisolone aceponate monohydrate is substantially represented by the detailed spectrogram as figure 2. The methylprednisolone aceponate monohydrate can be prepared by a method of completely dissolving methylprednisolone aceponate in the mixed solution of water and an organic solvent and finally evaporating the organic solvent.

Description

Field of invention: [0001] The invention relates to a steroid compound, in particular to a new crystal form of methylprednisolone acetate and a preparation method thereof. Background technique: [0002] The chemical structure of methylprednisolone acetate (Methylprednisolone aceponate, MPA, CAS: 86401-95-8) is shown in the figure below: [0003] [0004] 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% methylprednisolone acetidine cream, which can be used to inhibit inflammation and allergic skin reactions, and also inhibit the accelerated regeneration of cells. Symptoms such as erythema, edema, thickening of the skin, subsidence of skin surface...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00A61K31/573A61P5/40
Inventor 何运良李静
Owner TIANJIN JINYAO GRP
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