Eureka AIR delivers breakthrough ideas for toughest innovation challenges, trusted by R&D personnel around the world.

Dasatinib crystal form and preparation method thereof

A technology for dasatinib and Nijing, which is applied in the field of dasatinib crystal form and preparation, can solve the problems that the solubility of the crystal form needs to be improved, the preparation process is cumbersome, and the solubility of the crystal form is low, and the preparation method is simple and feasible, Excellent physical and chemical properties and stable product

Active Publication Date: 2020-03-06
LUNAN PHARMA GROUP CORPORATION
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN201210314388.3 discloses a dasatinib polymorph III, but its preparation process is cumbersome, and the treatment of industrialized organic waste liquid is increased, and the solubility of the crystal form is low
201110316498.9 discloses a new crystal form III of dasatinib monohydrate. Although the preparation process is simple, the solubility of the obtained crystal form needs to be improved, and the dissolution rate is low
In the prior art, the solubility and stability of dasatinib crystal form need to be further improved

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
  • Dasatinib crystal form and preparation method thereof
  • Dasatinib crystal form and preparation method thereof
  • Dasatinib crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Add the crude product monohydrate of dasatinib into the absolute ethanol solution, wherein the concentration of dasatinib in the absolute ethanol solution is 0.1mg / mL;

[0044] (2) Ultrasonic heating was carried out in a desktop ultrasonic instrument to dissolve it, and the temperature was 35°C for 20 minutes;

[0045] (3) Slowly cool down to 0°C, filter, place in a small beaker, seal with parafilm, prick holes, volatilize, and crystallize for 20 minutes;

[0046] (4) Filtrate and dry under reduced pressure at 50°C to obtain a single crystal of dasatinib.

[0047] The product yield is 85.7%, and the product purity is 99.91%. After determination, its X-ray powder diffraction pattern and figure 1 Basically the same.

Embodiment 2

[0049] (1) Dasatinib monohydrate is added to the absolute ethanol solution, wherein the concentration of dasatinib in the absolute ethanol solution is 7 mg / mL;

[0050] (2) Ultrasonic heating is carried out in a desktop ultrasonic instrument to dissolve it, and the temperature is 45° C. for 1 hour;

[0051] (3) Slowly cool down to 35°C, filter, place in a small beaker, seal with parafilm, pierce holes, volatilize at room temperature, and crystallize for 10 hours;

[0052] (4) Filtrate and dry under reduced pressure at 40°C to obtain a single crystal of dasatinib.

[0053] The product yield is 90.5%, and the product purity is 99.98%. After determination, its X-ray powder diffraction pattern and figure 1 Basically the same.

Embodiment 3

[0055] (1) Dasatinib monohydrate was added to the absolute ethanol solution, wherein the concentration of dasatinib in the absolute ethanol solution was 9 mg / mL;

[0056] (2) Ultrasonic heating is carried out in a desktop ultrasonic instrument to dissolve it, and the temperature is 70° C. for 2 hours;

[0057] (3) Slowly cool down to 55°C, filter, place in a small beaker, seal with parafilm, prick holes, volatilize at room temperature, and crystallize for 48 hours;

[0058] (4) Filtrate and dry under reduced pressure at 60°C to obtain a single crystal of dasatinib.

[0059] The product yield is 88.8%, and the product purity is 99.95%. After determination, its X-ray powder diffraction pattern and figure 1 Basically the same.

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

PropertyMeasurementUnit
concentrationaaaaaaaaaa
concentrationaaaaaaaaaa
concentrationaaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of medicaments, and in particular to a dasatinib crystal form and a preparation method thereof. A powder diffraction spectrum of the dasatinib crystal formhas diffraction peaks at the positions with 2theta angles of 5.8+ / -0.2 degrees, 7.2+ / -0.2 degrees, 14.4+ / -0.2 degrees and 16.0+ / -0.2 degrees. The X-ray single crystal diffraction spectrum shows thatthe crystal form prepared by the method is an ethanol solvate crystal of dasatinib, purity of the crystal form is high, stability is good, and solubility is excellent. The crystal form particularly shows excellent dissolution performance in a dissolution experiment, has a preparation process which is easy to industrialize, and has a wide application prospect.

Description

technical field [0001] The invention relates to the technical field of medicines, in particular to a crystal form of dasatinib in the technical field and a preparation method thereof. Background technique [0002] Dasatinib, chemical name: N-(2-chloro-6-methylphenyl)-2-[[6-[4-(2-hydroxyethyl)-1-piperazinyl] -2-Methyl-4-pyrimidinyl]amino]-5-thiazolecarboxamide, molecular formula is C22H26C1N7O2S, molecular weight is 488.00600, CAS863127-77-9. Dasatinib is an antineoplastic drug, whose trade name is SPRYCEL. It is an oral tyrosine kinase inhibitor developed by BMS. It is mainly used to treat imatinib mesylate resistance or intolerance clinically. Adult patients with Philadelphia chromosome positive (Ph+) chronic myeloid leukemia (CML) in chronic phase, accelerated phase, and blast phase (myeloid and lymphocytic changes). [0003] The chemical structure is as follows: [0004] [0005] Different crystal forms can exhibit different chemical and physical properties, which h...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12A61P35/00A61K31/506
CPCC07D417/12A61P35/00C07B2200/13
Inventor 张贵民翟立海张明明郭立红
Owner LUNAN PHARMA GROUP CORPORATION
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
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