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Method for detecting purity of 3-chloromethyl-1, 2, 4-triazolin-5-one

A detection method, chloromethyl technology, applied in the field of analysis, can solve problems such as undiscovered, and achieve the effect of improving accuracy and speed of detection

Inactive Publication Date: 2021-03-12
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the process of preparing aprepitant, the detection of the purity and impurity content of 3-chloromethyl-1,2,4-triazolin-5-one is particularly important, but 3-chloromethyl-1,2,4-one has not been found in the prior art Relevant literature and reports on the detection method of the purity and impurity content of methyl-1,2,4-triazolin-5-one

Method used

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  • Method for detecting purity of 3-chloromethyl-1, 2, 4-triazolin-5-one
  • Method for detecting purity of 3-chloromethyl-1, 2, 4-triazolin-5-one
  • Method for detecting purity of 3-chloromethyl-1, 2, 4-triazolin-5-one

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Experimental program
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Embodiment 1

[0042] Embodiment 1: The detection method of 3-chloromethyl-1,2,4-triazolin-5-one purity

[0043] A method for detecting the purity of 3-chloromethyl-1,2,4-triazolin-5-one, comprising the following steps:

[0044] The blank test is: the diluent (the diluent is KH 2 PO 4 80:20 mixture of buffer and acetonitrile by volume, KH 2 PO 4 The pH of buffer solution is 3) detect with liquid chromatography, record chromatogram C,

[0045] Dissolve 3-chloromethyl-1,2,4-triazolin-5-one in diluent (diluent is KH 2 PO 4 80:20 mixture of buffer and acetonitrile by volume, KH 2 PO 4 When the pH of the buffer is 3), a control sample solution is obtained. In the control sample solution, the concentration of 3-chloromethyl-1,2,4-triazolin-5-one is 0.5 mg / mL;

[0046] The test sample 1 containing 3-chloromethyl-1,2,4-triazolin-5-one is dissolved in the diluent (the diluent is KH 2 PO 4 80:20 mixture of buffer and acetonitrile by volume, KH 2 PO 4The pH of buffer solution is 3), obtains...

Embodiment 2

[0066] Embodiment 2: The detection method of the purity of 3-chloromethyl-1,2,4-triazolin-5-one

[0067] The difference between embodiment 2 and embodiment 1 is that the test sample 1 is replaced by the test sample 2, and the rest of the process is the same. The area normalization method was used to calculate the purity and impurity content of 3-chloromethyl-1,2,4-triazolin-5-one in the test sample 2, and the results are shown in Table 2.

[0068] Table 2

[0069]

[0070]

[0071] As can be seen from Table 2, the purity of 3-chloromethyl-1,2,4-triazolin-5-one in sample 2 to be tested reaches 99.12%, the maximum single impurity content reaches 0.50%, and the total impurity content reaches 0.88% %.

Embodiment 3

[0072] Embodiment 3: The detection method of the purity of 3-chloromethyl-1,2,4-triazolin-5-one

[0073] The difference between embodiment 3 and embodiment 1 is that the test sample 1 is replaced by the test sample 3, and the rest of the process is the same. The area normalization method was used to calculate the purity and impurity content of 3-chloromethyl-1,2,4-triazolin-5-one in the test sample 3, and the results are shown in Table 3.

[0074] image 3 It is the chromatogram B obtained in the detection method of Example 3. image 3 "4" in represents the peak corresponding to 3-chloromethyl-1,2,4-triazolin-5-one, image 3 "1" in represents the peak corresponding to "maximum simple heterogeneity", image 3 "2" and "3" in represent the corresponding peaks of other impurities ( image 3 The ordinate "Absorbance" in the graph represents absorbance, the unit is mAU, and the abscissa represents time, the unit is min, that is, minutes).

[0075] table 3

[0076]

[0077] ...

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Abstract

The invention belongs to the technical field of analysis, and discloses a method for detecting the purity of 3-chloromethyl-1, 2, 4-triazoline-5-one. The detection method comprises the following steps: dissolving 3-chloromethyl-1, 2, 4-triazoline-5-one in a diluent to obtain a control sample solution; dissolving a to-be-detected sample in the diluent to obtain a to-be-detected sample solution; taking the control sample solution, detecting by liquid chromatography, and recording a chromatogram A; taking the to-be-detected sample solution, detecting the to-be-detected sample solution by liquid chromatography, and recording a chromatogram B; and calculating the purity according to the chromatogram A and the chromatogram B. The conditions of the liquid chromatography comprise a mobile phase Aand a mobile phase B; the mobile phase A is a phosphate buffer solution and acetonitrile; the mobile phase B is acetonitrile; and the volume ratio of the phosphate buffer solution to acetonitrile in the mobile phase A is (950 + / -5): (50 + / -0.5). The detection method can accurately detect the purity of the 3-chloromethyl-1, 2, 4-triazoline-5-one in the to-be-detected sample.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a detection method for the purity of 3-chloromethyl-1,2,4-triazolin-5-one. Background technique [0002] Aprepitant is clinically mainly used to prevent acute and delayed nausea and vomiting during the initial and repeated treatment of highly emetogenic anticancer chemotherapy. 3-Chloromethyl-1,2,4-triazolin-5-one, whose CAS number is 252742-72-6, 3-chloromethyl-1,2,4-triazolin-5-one is The important intermediate for producing aprepitant, the purity and impurity content of 3-chloromethyl-1,2,4-triazolin-5-one directly affect the purity and impurity content of aprepitant, thus directly Affect the drug efficacy of aprepitant. [0003] In the process of preparing aprepitant, the detection of the purity and impurity content of 3-chloromethyl-1,2,4-triazolin-5-one is particularly important, but 3-chloromethyl-1,2,4-one has not been found in the prior art Relevant liter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/74G01N30/8679
Inventor 蒙发明罗凤玲陈舒婷张伟鹏
Owner ENANTIOTECH CORP
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