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2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form and preparation method thereof

A technique for methosulide crystal and crystallization, applied in the field of methosulide crystal form and preparation thereof

Active Publication Date: 2014-02-05
WUHAN OPTICS VALLEY HUMANWELL BIO PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, impurities may lead to unwanted physicochemical properties such as: hygroscopicity or pharmacological side effects, etc.

Method used

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  • 2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form and preparation method thereof
  • 2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form and preparation method thereof
  • 2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation Mesosulide

[0045] Add 2-(4'-methoxyphenoxy)-methanesulfonanilide and acetic acid into the reaction kettle, stir, after completely dissolving, add nitric acid, after the reaction is completed, cool at room temperature, and collect the precipitated yellow Solid, washed with water until neutral, dried to obtain crude Mesosulide. The crude product was recrystallized with ethanol, heated to reflux and filtered, then crystallized naturally, the solid was collected by filtration, and dried in vacuo to obtain light yellow crystals or crystalline powder, i.e. mesosulide, with a yield of 60.4%. Qualified samples of mesosulide produced in three consecutive batches of pilot scale scale-up,

[0046] Batch number: 20120202 (analysis number W20120237-7),

[0047] 20120314 (analysis number W20120237-8),

[0048] 20120316 (Assay No. W20120237-9).

Embodiment 2

[0050] Mesosulide batch number: 20120509-1 (analysis number W20120237-1): Take 1g of crude mesosulide in a 50ml single-mouth bottle, put it into a magnet, add 20ml of ethanol, heat and reflux for 2h to completely dissolve, cool and crystallize, Filter, dry, and send for inspection.

[0051] figure 1 It is the X-ray diffraction experimental conditions and diffraction pattern of the above-mentioned mesosulide crystal with batch number 20120509-1 (analysis number W20120237-1);

[0052] figure 2 yes figure 1 The relevant data of the X-ray diffraction peak in;

[0053] Figure 4 It is the DSC chart of the above-mentioned mesosulide crystal with batch number 20120509-1 (analysis number W20120237-1).

Embodiment 3

[0055] Methosulide batch number: 20120509-3 (analysis number W20120237-2): Take 1g of crude mesosulide in a 50ml single-mouth bottle, put it into a magnet, add 20ml of methanol, heat and reflux for 2h to completely dissolve, cool and crystallize, Filter, rinse with ethanol, rinse with ethanol, dry, and send for inspection.

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Abstract

The invention provides a 2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form and a preparation method thereof. In an X-ray powder diffraction pattern of the 2-(4'-methoxy phenoxy)-4-nitro methanesulfonanilide crystal form, X-ray diffraction peaks appear at 2 theta of 11.6+ / -0.2 DEG, 17.9+ / -0.2 DEG and 21.4+ / -0.2 DEG. The crystal form has high purity.

Description

technical field [0001] The invention relates to the field of crystal forms of compounds, in particular to a crystal form of mesosulide and a preparation method thereof. Background technique [0002] Mesosulide, the chemical name is 2-(4'-methoxyphenoxy)-4-nitromethanesulfonanilide, and its structural formula is as follows: [0003] [0004] Mesosulide is a non-steroidal anti-inflammatory drug with good anti-inflammatory, analgesic and antipyretic effects. Previous research on mesosulide found that some impurities in the final product were not easy to remove, and no further research was done on the crystal form of the compound. Those skilled in the art are well aware of the need for high purity compounds in the pharmaceutical field. High purity improves long-term storage stability. On the other hand, impurities may lead to unwanted physicochemical properties such as hygroscopicity or pharmacological side effects, etc. [0005] Therefore, further in-depth research on me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/08C07C303/44
Inventor 王学海李莉娥许勇江曦乐洋朱垒胡虹杨仲文王磊周欢沈洁
Owner WUHAN OPTICS VALLEY HUMANWELL BIO PHARMA
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