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Crystal form A of gefitinib and method for preparing gefitinib

A kind of production technology and crystal form technology, which is applied in the field of biomedicine, can solve the problems of drug content, drug crystal form cannot be reproduced, low purity of the product, and poor method reproducibility, so as to achieve easy control of product quality, easy purchase, and environmental pollution. small effect

Inactive Publication Date: 2017-02-22
WUHAN DENUOMEI BIOLOGY MEDICINE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the preparation method of CN104418812A at present, the obtained Renji product has low purity and high impurity content; the method has poor reproducibility, and it is difficult to scale up to a pilot scale, so that the content of the drug and the crystal form of the drug cannot be reproduced

Method used

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  • Crystal form A of gefitinib and method for preparing gefitinib
  • Crystal form A of gefitinib and method for preparing gefitinib
  • Crystal form A of gefitinib and method for preparing gefitinib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] Embodiment 1: compound shown in preparation formula 2

[0092] Add 5kg of the compound shown in Formula 1, 55kg of acetic acid, and 50L of tetrahydrofuran into a 500L reactor, start stirring; add 6kg of iron powder, heat up to 40-45°C and keep it warm for 3 hours, and the reaction is complete by sampling and spotting. (TLC detection: silica gel GF254 thin-layer plate; developing agent: petroleum ether / ethyl acetate=1:2) the above reaction mixture was cooled to 25~35° C., and ethyl acetate (EA) (EA) ( 10 times, v / m), stirring for 30 minutes. Filter, and rinse the filter cake with ethyl acetate 2 to 3 times. The filtrate was transferred to a 500L reactor, and 10 times the volume of 10% sodium chloride solution was added, stirred for 5 minutes, and a green solid was precipitated, left to stand for 5 to 10 minutes, and the lower layer of water phase was released, and 10 times the volume of 10% chlorine was added. Sodium chloride solution, stirring for 5 minutes, standing ...

Embodiment 2

[0093] Embodiment 2: compound shown in preparation formula 2

[0094] Add 8kg of the compound shown in Formula 1, 84kg of acetic acid, and 80L of tetrahydrofuran into a 500L reactor, start stirring; add 11.2kg of iron powder, heat up to 45-50°C and keep it warm for 1.5 hours, and the reaction is complete by sampling and spotting. (TLC detection: silica gel GF254 thin-layer plate; developing agent: petroleum ether / ethyl acetate=1:2) the above reaction mixture was cooled to 25~35° C., and ethyl acetate (EA) (EA) ( 10 times, v / m), stirring for 30 minutes. Filter, and rinse the filter cake with ethyl acetate 2 to 3 times. The filtrate was transferred to a 500L reactor, and 10 times the volume of 10% sodium chloride solution was added, stirred for 5 minutes, and a green solid was precipitated, left to stand for 5 to 10 minutes, and the lower layer of water phase was released, and 10 times the volume of 10% chlorine was added. Sodium chloride solution, stirring for 5 minutes, stan...

Embodiment 3

[0095] Embodiment 3: compound shown in preparation formula 2

[0096] Add 8kg of the compound shown in Formula 1, 80kg of acetic acid, and 78L of tetrahydrofuran into a 500L reactor, start stirring; add 10kg of iron powder, heat up to 50-55°C and keep it warm for 2 hours, and the reaction is complete by sampling and spotting. (TLC detection: silica gel GF254 thin-layer plate; developing agent: petroleum ether / ethyl acetate=1:2) the above reaction mixture was cooled to 25~35° C., and ethyl acetate (EA) (EA) ( 10 times, v / m), stirring for 30 minutes. Filter, and rinse the filter cake with ethyl acetate 2 to 3 times. The filtrate was transferred to a 500L reactor, and 10 times the volume of 10% sodium chloride solution was added, stirred for 5 minutes, and a green solid was precipitated, left to stand for 5 to 10 minutes, and the lower layer of water phase was released, and 10 times the volume of 10% chlorine was added. Sodium chloride solution, stirring for 5 minutes, standing...

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Abstract

The invention discloses a crystal form A of gefitinib and a method for preparing the gefitinib. In an X-ray powder diffraction spectrum of the crystal form A of the gefitinib, peaks exist at the following 2theta angles: 7.38+ / -0.2 degrees, 11.40+ / -0.2 degrees, 14.72+ / -0.2 degrees, 16.59+ / -0.2 degrees and 26.80+ / -0.2 degrees. A novel crystal form A product of the gefitinib is high in purity and has the good physical and chemical stability.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, in particular, the invention relates to the crystal form A of rengui and a method for preparing rengui. Background technique [0002] Renguitar (also known as mefitinib, chemical name: 6-(3-acetoxymethyl-3-methyltriazene)-4-(3-chlorophenylamino)quinazoline) as a target An innovative drug for the treatment of cancer, it is a selective epidermal growth factor receptor (EGFR) tyrosine kinase inhibitor. However, according to the preparation method of CN104418812A at present, the obtained Rengui product has low purity and high impurity content; the method has poor reproducibility, and it is difficult to scale up to a pilot scale, so that the content of the drug and the crystal form of the drug cannot be reproduced. [0003] Therefore, the new crystal form of rengui and the method for preparing rengui still need to be further improved. Contents of the invention [0004] The present invention ai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/94
CPCC07D239/94C07B2200/13
Inventor 全欣鑫邱启裕
Owner WUHAN DENUOMEI BIOLOGY MEDICINE TECH
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