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Crystal form of quinazoline compound and preparation method thereof

A technology for quinazolines and compounds, which is applied in the field of crystal forms of quinazolines and their preparation, and can solve problems such as excessive cell proliferation

Active Publication Date: 2020-05-15
GUANGZHOU LIUSHUN BIO TEC CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sustained signaling leads to hyperproliferation of cells, thus leading to tumorigenesis and progression

Method used

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  • Crystal form of quinazoline compound and preparation method thereof
  • Crystal form of quinazoline compound and preparation method thereof
  • Crystal form of quinazoline compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0122] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:

[0123] (1) The crude product 3.00g of quinazoline compound is washed 2 times with purified water (4.65g), ethanol (1.90g), after controlling vacuum-0.08MPa temperature 20 ℃ of drying 2 hours in vacuum oven, then heat up Dry at 50°C for 20 hours, take out the solid, then add 38.0g of dimethyl sulfoxide (DMSO) to 40°C and stir to dissolve, filter, add purified water (70g) and stir, and then filter;

[0124] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 78°C with 37.0g of ethanol for beating under reflux for 3 hours, cooled to 20°C for filtration, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 78°C, continue stirring for 3h, drop to 20°C and fi...

Embodiment 2

[0127] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:

[0128] (1) 3.00 g of the crude product of quinazoline compounds are washed twice with purified water (4.65 g), ethanol (1.90 g), and after drying for 2 hours at a temperature of 30° C. of vacuum-0.10 MPa in a vacuum oven, the temperature is raised Dry at 55°C for 20 hours, take out the solid, then add 38.0g of dimethyl sulfoxide (DMSO) to 45°C and stir to dissolve, filter, add purified water (70g) and stir, and then filter;

[0129] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 70°C with 37.0g of ethanol to reflux for beating for 2 hours, cooled to 20°C for filtration, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 83°C, continue to stir for...

Embodiment 3

[0132] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:

[0133] (1) The crude product 3.00g of quinazoline compound is washed 2 times with purified water (4.65g), ethanol (1.90g), after controlling vacuum-0.09MPa temperature 20 ± 10 ℃ of drying 2 hours in vacuum oven, Then raise the temperature to 45°C and dry for 20 hours, take out the solid, then add 38.0 g of dimethyl sulfoxide (DMSO) and stir to dissolve at 35°C, filter, add purified water (70 g) and stir, and then filter;

[0134] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 80° C. for reflux with 37.0 g of ethanol for beating for 5 hours, cooled to 20° C., filtered, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 72°C, continue stirring for ...

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Abstract

The invention relates to a crystal form of a quinazoline compound and a preparation method thereof, and belongs to the technical field of biological medicines. The compound can be used as a multi-target-point kinase inhibitor. The invention provides a crystal form of a quinazoline compound with higher stability. The structural formula of the quinazoline compound is shown as a formula (I), and theX-ray powder diffraction pattern 2[theta] diffraction angles of the quinazoline compound crystal forms A, Form1, Form2, Form3, Form4, Form5, Form6, Form7 and Form8 have characteristic diffraction peaks at 3-40 degrees; the preparation method of the crystal form of the quinazoline compound provided by the invention has an important value for optimization and development of the medicine, the preparation method is simple and easy to operate, the process purification effect is remarkable, the used solvent has small harm to the environment and is suitable for industrial production; and the crystalform A of the quinazoline compound provided by the invention has good stability and reproducibility, is convenient to transfer, store and operate in a production process in the future, and is safer inclinical medication.

Description

technical field [0001] The invention relates to a crystal form of a quinazoline compound and a preparation method thereof. The compound has the function of a multi-target kinase inhibitor and belongs to the technical field of biomedicine. Background technique [0002] Cells contain complex signal transduction pathways, which are mediated by tyrosine protein kinases and involve changes in the structure and function of many proteins in the human body. Abnormal signal transduction of cells is one of the key factors in the occurrence and development of tumors. The target of tyrosine protein kinase has been a hotspot in the research of anticancer drugs in recent decades. With the deepening of research and the clinical application of drugs, it is found that the therapeutic effect of blocking the specific signal transduction pathway of tumor cells through single-target drugs may not be objective enough, and there is a resistance to the activation of bypass compensatory signaling pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/88
CPCC07B2200/13C07D239/88
Inventor 刘兵戴静思王嫣董俊军钱学启王思明陈能安邓联武
Owner GUANGZHOU LIUSHUN BIO TEC CO LTD
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