Method for preparing large particle size dasatinib

A technology of dasatinib and large particle size, which is applied in the field of preparing large particle size dasatinib, can solve the problems of increased preparation cost, large loss, long time consuming for filtration and washing treatment, etc., and achieves lower production cost and better flow rate Compressibility and compressibility, the effect of moderate solubility

Active Publication Date: 2013-12-25
SHANGHAI ACEBRIGHT PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in the filtration and separation process, the filtration and washing of small particles takes a long time and consumes a lot, which easily leads to an increase in the preparation cost, which is not conducive to the requirements of industrial production.

Method used

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  • Method for preparing large particle size dasatinib
  • Method for preparing large particle size dasatinib
  • Method for preparing large particle size dasatinib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 10 g of dasatinib and 300 ml of absolute ethanol to a 500 ml four-necked flask equipped with a mechanical stirrer, a condenser and a thermometer to obtain a slurry; heat and reflux to 75° C. to obtain a clear solution; then, slowly cool the solution to 60 °C to obtain a suspension; then slowly cool down to room temperature for 10 hours, filter, and dry the obtained solid at 50 °C to obtain 8.9 g of a dry product. The particle size is: D (0.1) = 3.4 μm , D(0.5)=20.1 μm, D(0.9)=130.2 μm.

Embodiment 2

[0034] Add 10 g of dasatinib and 300 ml of absolute ethanol to a 500 ml four-necked flask equipped with a mechanical stirrer, a condenser and a thermometer to obtain a slurry; heat and reflux to 75° C. to obtain a clear solution; then, slowly cool the solution to 60 °C to obtain a suspension; heat the suspension to 60-65 °C, then cool to 55 °C; keep warm at 55 °C and stir for 1 hour; heat to 65 °C again; slowly cool down to room temperature after 4 hours, filter, and The obtained solid was dried at 50° C. to obtain 9.1 g of a dry product, and its particle size was found to be: D(0.1)=6.4 μm, D(0.5)=55.2 μm, D(0.9)=140.3 μm.

Embodiment 3

[0036] Add 20 g of dasatinib and 700 ml of acetone to a 1000 ml four-necked flask equipped with a mechanical stirrer, a condenser and a thermometer to obtain a slurry; heat to reflux to 56° C. to obtain a clear solution; then, slowly cool the solution to 48° C. The suspension was obtained, and then slowly cooled to room temperature after 5 hours, the solution was filtered, and the obtained solid was dried at 50° C. to obtain 18.5 g of a dry product. The particle size was determined to be: D(0.1)=4.2 μm, D(0.5)=50.1 μm, D(0.9)=137.1 μm.

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Abstract

The invention discloses a method for preparing large particle size dasatinib, which comprises the following steps of: adding dasatinib into an organic solvent to obtain slurry; heating until backflow to obtain a clear solution; cooling the solution to decrease the temperature by 5-15 DEG C to obtain a suspension; cooling the suspension for 5-15 h to room temperature; and filtering the suspension, and vacuum-drying the obtained solid at 40-60 DEG C. Large particle size dasatinib with particle sizes D (0.1)=3.0 to 10 mum, D (0.5)=15 to 60 mum and D (0.9)=100 to 150 mum can be obtained by using the preparation method provided by the invention. Experiments prove that dasatinib obtained in the invention has good flowability and compressibility and moderate solubility and is beneficial to making of qualified preparations and lowering the production cost of raw materials and preparations, and the requirement of industrial production can be satisfied.

Description

technical field [0001] The invention relates to a method for preparing dasatinib with large particle size, belonging to the technical field of organic chemistry. Background technique [0002] Dasatinib, the chemical name is N-(2-chloro-6-methylphenyl)-2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methanol Base pyrimidin-4-yl]amino]-1,3-thiazole-5-carboxamide, the molecular formula is C 22 h 28 ClN 7 o 3 S, the molecular weight is 488.01, and its chemical structure is as follows: [0003] [0004] Dasatinib is a potent oncogenic kinase inhibitor developed by Bristol-Myers Squibb, which has been clinically used to treat various stages of chronic myeloid leukemia, Philadelphia chromosome-positive acute lymphoblastic leukemia and solid treatment of tumor patients. [0005] Chinese patent CN200580011916.6 discloses five crystalline forms of dasatinib (monohydrate, butanol solvate, ethanol solvate, N-6 in pure form, TIHI-7 in pure form) and discloses Methods for the prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/12
Inventor 安晓霞吕锋申淑匣
Owner SHANGHAI ACEBRIGHT PHARMA CO LTD
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