Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF7 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 gefitinib prepared in the examples is in the range of 119°C to 120°C. It is determined that its crystal form is different from the Form 1 polymorph discovered later, presumably as A metastable crystalline form for which no X-ray diffraction (XRPD) pattern is disclosed

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com