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A crystalline form of a cyclin-dependent protein kinase inhibitor and a preparation method thereof

A crystallization and solvent technology, used in organic chemical methods, pharmaceutical formulations, organic active ingredients, etc., can solve the problems of easy agglomeration, poor product stability, difficult filtration, etc., and achieve repeatable and controllable production processes and crystal stability. Good, stable production process effect

Active Publication Date: 2019-03-12
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, amorphous drug products have no regular crystal structure and often have other defects, such as poor product stability, fine crystallization, difficult filtration, easy agglomeration, poor fluidity, etc.

Method used

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  • A crystalline form of a cyclin-dependent protein kinase inhibitor and a preparation method thereof
  • A crystalline form of a cyclin-dependent protein kinase inhibitor and a preparation method thereof
  • A crystalline form of a cyclin-dependent protein kinase inhibitor and a preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take (1.0g, 2.24mmol) the compound represented by formula (I) (prepared according to the method provided by WO2014183520) and add it to a 250ml Erlenmeyer flask, add 40ml ethanol, stir at room temperature, then drop dilute hydrochloric acid (219mg, 6.01mmol) (dissolved in 4ml of water), heated to 60°C, dissolved, dropped into sodium bicarbonate solution (1.21g, 14.40mmol) (dissolved in 40ml of water), cooled to room temperature and stirred overnight. After drying, 0.89 g of solid was obtained, and the yield was 89.0%. The X-ray diffraction spectrum figure of this crystalline sample is shown in figure 1 . The crystallization at about 4.91 (17.99), 9.91 (8.92), 10.53 (8.39), 14.82 (5.98), 16.04 (5.52), 17.34 (5.11), 18.51 (4.79), 19.92 (4.45), 21.19 (4.19), 22.65 (3.92), 24.15(3.68), 26.92(3.31), and 28.98(3.08) have characteristic peaks. See the DSC spectrum figure 2 , with a sharp melting endothermic peak at 289.22°C, this crystal form is defined as I crystal form....

Embodiment 2

[0036] Get (1.0g, 2.24mmol) compound shown in formula (I) (prepared by Example 1) and join in the 250ml Erlenmeyer flask, add 40ml methanol, stir at room temperature, drop dilute hydrochloric acid (219mg, 6.01mmol) then ( dissolved in 4ml of water), heated to 60°C, dissolved, dropped into sodium bicarbonate solution (1.21g, 14.40mmol) (dissolved in 40ml of water), cooled to room temperature and stirred overnight. After drying, 0.98 g of solid was obtained, and the yield was 98.0%. Its X-diffraction and DSC patterns are researched and compared, and it is confirmed that the product is I crystal form.

Embodiment 3

[0038] Get (1.0g, 2.24mmol) the compound shown in formula (I) (prepared by Example 1) and join in the 250ml Erlenmeyer flask, add 40ml isopropanol, stir at room temperature, then drop dilute hydrochloric acid (219mg, 6.01mmol ) (dissolved in 4ml of water), heated to 60°C, dissolved, dropped into sodium bicarbonate solution (1.21g, 14.40mmol) (dissolved in 40ml of water), cooled to room temperature and stirred overnight. After drying, 0.52 g of solid was obtained, and the yield was 52.0%. Its X-diffraction and DSC patterns are researched and compared, and it is confirmed that the product is I crystal form.

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Abstract

The invention relates to a crystal form of a cyclin dependent protein kinase inhibitor and a preparation method thereof. Specifically, the invention relates to a type I crystal of a cyclin dependent protein kinase (CDK4&6) inhibitor and a preparation method thereof. Specifically, the invention relates to a type I crystal of 6-acetyl-8-cyclopentyl-5-methyl-2-((5-(piperidine-4-yl)pyridine-2-yl)amino)pyridine[2, 3-d]pyrimidine-7(8H)-one (formula (I) compound) and a preparation method thereof, wherein the crystal has an X-ray powder diffraction spectrum shown as Figure 1. The type I crystal of the formula (I) compound obtained by the invention has good chemical stability and crystal form stability, and the used crystal solvent has low toxicity and low residue, thus being better applicable to clinical treatment. (formula (I)).

Description

technical field [0001] The present invention relates to 6-acetyl-8-cyclopentyl-5-methyl-2-((5-(piperidin-4-yl)pyridin-2-yl)amino)pyrido[2,3-d] Pyrimidin-7(8H)-one and its I crystal form. The compound of formula (I) prepared according to the method of the present invention can be used for the treatment of breast cancer. Background technique [0002] Breast cancer is one of the most common malignant tumors in women. It has a high incidence rate and is quite invasive, but the course of the disease progresses slowly. On February 1, 2010, the China Population Association released the "China Breast Disease Survey Report" in Beijing. The report shows that, The mortality rate of breast cancer in my country's urban areas has increased by 38.91%. Breast cancer has become the most threatening disease to women's health. Currently, there are at least 156 breast cancer drugs under research and on the market, of which 68% are targeted therapy drugs. A large number of studies It was found t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04A61K31/519A61P35/00
CPCC07B2200/13C07D471/04
Inventor 武乖利郭昌山边林卢韵沈灵佳
Owner JIANGSU HENGRUI MEDICINE CO LTD
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