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Method for detecting crizotinib intermediate

A technology of crizotinib and detection method, which is applied in the field of analysis, can solve the problems of not finding crizotinib intermediates, etc., and achieve the effect of improving separation effect, high applicability, and improving accuracy and reproducibility

Active Publication Date: 2020-07-31
ENANTIOTECH CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are no related literatures and reports on enantiomer detection methods of crizotinib intermediates

Method used

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  • Method for detecting crizotinib intermediate
  • Method for detecting crizotinib intermediate
  • Method for detecting crizotinib intermediate

Examples

Experimental program
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Embodiment 1

[0084] This embodiment provides a detection method for crizotinib intermediates, comprising the following steps:

[0085] (1) Dissolve the racemate of crizotinib intermediate 1 in an organic solvent to obtain a control sample solution A1; dissolve the crizotinib intermediate 1 to be tested in an organic solvent to obtain a test sample solution B1 ;

[0086] The organic solvent is formed by mixing n-hexane, isopropanol and diethylamine in a volume ratio of 50:50:0.5. The concentration of control sample solution A1 and test sample solution B1 is 0.5mg / mL.

[0087] (2) Get described control sample solution A1, inject liquid chromatograph, record the chromatogram of control sample A1.

[0088] (3) get described test sample solution B1, inject liquid chromatograph, record the chromatogram of test sample B1, calculate the percentage of enantiomer by area normalization method, the results are shown in Table 1 and figure 1 .

[0089] The chromatographic conditions in the present emb...

Embodiment 2

[0103] This embodiment provides a detection method for crizotinib intermediates, comprising the following steps:

[0104] (1) control sample solution is the same as embodiment 1; Crizotinib intermediate 2 to be tested is dissolved in an organic solvent to obtain test sample solution B2;

[0105] The organic solvent is formed by mixing n-hexane, isopropanol and diethylamine in a volume ratio of 50:50:0.5. The concentration of control sample solution A1 and test sample solution B2 is 0.5mg / mL.

[0106] (2) get described test sample solution B2, inject liquid chromatograph, record the chromatogram of test sample B2, calculate the percentage of enantiomer by area normalization method, the results are shown in Table 2 and figure 2 .

[0107] The chromatographic conditions in the present embodiment are:

[0108] Chromatographic column: chiralcel AD-H (4.6*250mm, 5μm);

[0109] Injection volume: 20μL;

[0110] Flow rate: 1.0mL / min;

[0111] Column temperature: room temperature...

Embodiment 3

[0120] This embodiment provides a detection method for crizotinib intermediates, comprising the following steps:

[0121] (1) control sample solution is the same as embodiment 1; Crizotinib intermediate 3 to be tested is dissolved in an organic solvent to obtain test sample solution B3;

[0122] The organic solvent is formed by mixing n-hexane, isopropanol and diethylamine in a volume ratio of 50:50:0.5. The concentration of control sample solution A1 and test sample solution B3 is 0.5mg / mL.

[0123] (2) get described test sample solution B3, inject liquid chromatograph, record the chromatogram of test sample, calculate the percentage of enantiomer by area normalization method, the results are shown in Table 3 and image 3 .

[0124] The chromatographic conditions in the present embodiment are:

[0125] Chromatographic column: chiralcel AD-H (4.6*250mm, 5μm);

[0126] Injection volume: 20μL;

[0127] Flow rate: 1.0mL / min;

[0128] Column temperature: room temperature;

...

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Abstract

The invention relates to a method for detecting a crizotinib intermediate. The method comprises the following steps: dissolving a crizotinib intermediate racemate in an organic solvent to obtain a control sample solution; dissolving the crizotinib intermediate to be detected in the organic solvent to obtain a test sample solution; taking the control sample solution, detecting by liquid chromatography, and recording a chromatogram A; taking the to-be-tested sample solution, detecting the to-be-tested sample solution by liquid chromatography, and recording a chromatogram B; and calculating according to the chromatogram A and the chromatogram B, wherein the structural formula of the crizotinib intermediate is represented by formula (1). The detection method is simple to operate, is not influenced by sample batches, has high applicability, and can accurately, quickly and reliably obtain the enantiomer content of the crizotinib intermediate.

Description

technical field [0001] The invention relates to the field of analysis, in particular to a method for detecting an intermediate of crizotinib. Background technique [0002] Crizotinib, chemical name 3-[(R)-1-(2,6-dichloro-3-fluorophenyl)ethoxy]-5-[1-(piperidin-4-yl)- 1H-pyrazol-4-yl]pyridin-2-amine, its structural formula is shown in formula 1-1. Crizotinib is an oral targeted drug for the treatment of NSCLC, which is a drug targeting the fusion gene (EML4-ALK) formed by echinoderm microtubule binding protein 4 and anaplastic lymphoma kinase. The drug was approved by the U.S. FDA in 2011 as a small molecule targeted drug for the treatment of advanced NSCLC patients with positive anaplastic lymphoma kinase (ALK). [0003] [0004] An important intermediate is involved in the preparation of crizotinib, the chemical name is (S)-1-(2,6-dichloro-3-fluorophenyl)ethanol, and its CAS number is 877397- 65-4, the structure of this intermediate is as follows: [0005] [0006]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34G01N2030/047Y02P20/55
Inventor 蒙发明陈舒婷甘鑫钰李胜辉
Owner ENANTIOTECH CORP
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