New gefitinib crystal form and preparation method thereof

A gefitinib and crystal form technology, applied in the field of new crystal forms of anticancer drugs and their preparation, can solve the problems of not mentioning which crystal form of gefitinib exists, not disclosing X-ray diffraction methods, etc. , to achieve the effect of cheap and easy-to-obtain reagents, mild conditions and simple operation.

Active Publication Date: 2013-09-25
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] Astra Zenica Co., Ltd. applied for the compound patent CN96193526.X of gefitinib on April 23, 1996, which disclosed gefitinib and its hydrochloride, but did not mention gefitinib What kind of crystal form can gefitinib exist in? The melting point of gefit

Method used

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  • New gefitinib crystal form and preparation method thereof
  • New gefitinib crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 10.0g of gefitinib and 100ml of DMF into the reactor, dissolve at room temperature (about 25°C) for 30min, add 150ml of tert-butyl methyl ether anti-solvent, the system begins to crystallize, and crystallize at room temperature for 6h, filter and dry to obtain off-white solid 8.2g, the product was confirmed to be gefitinib α crystal form by XRPD and DSC analysis, with a purity of 99.5% and a yield of 82%.

Embodiment 2

[0038] 200ml of chloroform was used instead of 100ml of DMF, and other operations were performed according to Example 1 to obtain 8.1g of off-white solid. The product was confirmed to be Gefitinib α crystal form by XRPD and DSC analysis, with a purity of 99.5% and a yield of 81%.

Embodiment 3

[0040] 200ml of acetonitrile was used instead of 100ml of DMF, and the rest were operated according to Example 1 to obtain 8.1g of off-white solid. The product was confirmed to be Gefitinib α crystal form by XRPD and DSC analysis, with a purity of 99.5% and a yield of 81%.

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Abstract

The invention relates to a new crystal form alpha crystal form of gefitinib and a preparation method thereof. The crystal form has the strongest characteristic peak at a position where a 2theta angle is 7.12 on an X ray powder diffraction (XRPD) pattern, and has main characteristic peaks at positions where the 2theta angle are respectively 7.12, 24.349 and 26.435, wherein the relative strength of the main characteristic peaks are greater than 60%. The preparation method comprises: (a) adding gefitinib into a strong polarity solvent, and dissolving; (b) adding a smaller polarity anti-solvent into the solution, separating out crystals; (c) filtering, drying, and obtaining an almost white solid. The alpha crystal form is easy to prepare, good in stability and preparation formability, simple in preparation technology and mild in conditions; and the whole preparation process is carried out in 10 hours or less, so that the production efficiency is improved substantially, and the alpha crystal form is more suitable for industrialization production.

Description

technical field [0001] The invention relates to a new crystal form of an anticancer drug and a preparation method thereof, in particular to a new crystal form α of gefitinib and a preparation method thereof. Background technique [0002] Gefitinib, English name Gefitinib, developed by Astra Zenica Co., Ltd., trade name Iressa (IRESSA), is a selective epidermal growth factor receptor (EGFR) tyrosine kinase inhibitor , suitable for the treatment of locally advanced or metastatic non-small cell lung cancer (NSCLC) that has previously received chemotherapy or is not suitable for chemotherapy, and its structural formula is as follows: . [0003] Astra Zenica Co., Ltd. applied for the compound patent CN96193526.X of gefitinib on April 23, 1996, which disclosed gefitinib and its hydrochloride, but did not mention gefitinib What kind of crystal form can gefitinib exist in? The melting point of gefitinib prepared in the examples is in the range of 119°C to 120°C. It is determined...

Claims

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Application Information

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IPC IPC(8): C07D239/94
Inventor 张彦巧李晓芳孙文涛张素娟耿佳
Owner CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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