New Dasatinib crystal form and preparation method thereof

A dasatinib and crystal form technology, applied in the field of dasatinib-2-[[6-[4--1-piperazine, can solve the problems of no novelty and no application value, and achieve reproducibility Good performance, satisfying large-scale industrial production, and simple operation

Inactive Publication Date: 2015-02-11
SHANGHAI SYNCORES TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Patent WO2009053854 discloses 42 polymorphs of dasatinib, but most of them are solvent compounds and have no practical application value
[0010] In addition, the patent CN102086195 also discloses a polymorphic form of dasatinib, which is basically the same as the monohydrate crystal form and has no novelty

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] At room temperature, weigh 200mg of dasatinib free base, add it to 4ml of methanol solution, stir and suspend dasatinib in the solution system, add 1ml of 0.5M hydrochloric acid methanol solution dropwise to the suspension, and continue stirring until reaching Satinib is completely dissolved, and the filtrate is filtered for later use. Add 6ml of acetonitrile dropwise to the filtrate. After dripping, the solution is still clear. Then add 1ml of methanol containing 20mg of sodium hydroxide dropwise to the solution. After stirring for 5min, a solid precipitates out, continue stirring After 10 hours, filter and dry to obtain the new crystal form V of dasatinib.

Embodiment 2

[0039] At room temperature, weigh 200mg of dasatinib free base, add it to 4ml of ethanol solution, stir and suspend dasatinib in the solution system, add 1ml of 0.5M hydrochloric acid ethanol solution dropwise to the suspension, and continue stirring until reaching Satinib is completely dissolved, and the filtrate is filtered for later use. Add 6ml of acetonitrile dropwise to the filtrate. After dropping, the solution is still clear. Then add 1ml of ethanol containing 20mg of sodium hydroxide dropwise to the solution. After stirring for 5 minutes, solids precipitate out, and continue stirring. After 10 hours, filter and dry to obtain the new crystal form V of dasatinib.

Embodiment 3

[0041] At room temperature, weigh 200mg of dasatinib free base, add it to 5ml of isopropanol, stir and suspend dasatinib in the solution system, add 1ml of 0.5M isopropanol hydrochloride solution to the suspension, and continue stirring Until Dasatinib is completely dissolved, filter the filtrate for later use, add 6ml of ethyl acetate dropwise to the filtrate, after the drop, the solution is still clear, then add 1ml of isopropanol containing 20mg of sodium hydroxide dropwise to the solution, and stir for 5min Solids were precipitated, and the stirring was continued for 10 h, filtered and dried to obtain the new crystal form V of dasatinib.

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PUM

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Abstract

The invention relates to a new Dasatinib crystal form and a preparation method thereof. The new Dasatinib crystal form is named as a crystal form V and has characteristic peaks at 6.02 degrees, 6.91 degrees, 8.55 degrees, 12.44 degrees, 13.30 degrees, 13.84 degrees, 16.83 degrees, 24.41 degrees and 24.96 degrees (2theta) in an X ray powder diffraction spectrum obtained by means of Cu-Ka radiation detection. The invention also provides a method for preparing the new Dasatinib crystal form V. The method is simple, convenient and good in reproducibility, and the obtained new Dasatinib crystal form V is high in purity, good in stability and applicable to industrial production.

Description

technical field [0001] The present invention relates to dasatinib (N-(2-chloro-6-methylphenyl)-2-[[6-[4-(2-hydroxyethyl)-1-piperazine [0002] base]-2-methyl-4-pyrimidinyl]amino]-5-thiazole carboxamide) and its preparation method. technical background [0003] The chemical name of Dasatinib is N-(2-chloro-6-methylphenyl)-2-[[6-[4-(2-hydroxyethyl)-1-piperazinyl]-2-methyl -4-pyrimidinyl] amino]-5-thiazole carboxamide, the structural formula is as shown in formula I below: [0004] [0005] Formula Ⅰ [0006] Dasatinib, whose trade name is Sprycel, is a polytyrosine kinase inhibitor developed by Bristol-Myers Squibb. It is mainly used for the treatment of adult chronic myelogenous leukemia (CML), and can also treat other Treatment-resistant or intolerant adult patients with Philadelphia chromosome-positive acute lymphoblastic leukemia. [0007] Patent US6596746 discloses the compound preparation method of formula I, with 80%EtOH-H 2 The ethanol of O is heated and dissol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12
CPCC07D417/12C07B2200/13
Inventor 司永星方干许炜武文举张席妮
Owner SHANGHAI SYNCORES TECH INC
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