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Method for detecting purity of 2-(2-chloro-1-ethylene) hydrazide methyl formate

A technology of methyl hydrazide formate and a detection method, which is applied in the field of detection of the purity of methyl 2-hydrazide formate and can solve the problem of not finding the purity of methyl 2-(2-chloro-1-ethylene) hydrazide formate and the detection method of impurity content

Active Publication Date: 2021-04-20
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 methyl 2-(2-chloro-1-ethylidene) hydrazide formate is particularly important, but 2-(2 Relevant literature and reports on the detection method of the purity and impurity content of -chloro-1-ethylidene)hydrazide methyl formate

Method used

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  • Method for detecting purity of 2-(2-chloro-1-ethylene) hydrazide methyl formate
  • Method for detecting purity of 2-(2-chloro-1-ethylene) hydrazide methyl formate
  • Method for detecting purity of 2-(2-chloro-1-ethylene) hydrazide methyl formate

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Embodiment 1

[0045] Embodiment 1: the detection method of the purity of 2-(2-chloro-1-ethylene) methyl hydrazide formate

[0046] A method for detecting the purity of 2-(2-chloro-1-ethylene) hydrazide methyl formate, comprising the following steps:

[0047] 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,

[0048] Dissolve methyl 2-(2-chloro-1-ethylene)hydrazide formate 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 the buffer is 3), to obtain a control sample solution, in the control sample solution, the concentration of 2-(2-chloro-1-ethylidene)hydrazide methyl formate is 0.5mg / mL;

[0049] The test sample 1 containing 2-(2-chloro-1-ethylene) hydrazide methyl formate was dissolved in the diluent (the diluent was KH 2 PO 4 80:20 mixture of buffer and acetoni...

Embodiment 2

[0070] Embodiment 2: the detection method of the purity of 2-(2-chloro-1-ethylene) methyl hydrazide formate

[0071] 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 purity and impurity content of methyl 2-(2-chloro-1-ethylene)hydrazide formate in sample 2 to be tested were calculated by the area normalization method, and the results are shown in Table 2.

[0072] image 3 It is the chromatogram B obtained in the detection method of Example 2. image 3 "1" in represents the peak corresponding to methyl 2-(2-chloro-1-ethylene) hydrazide formate, image 3 "4" 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, and the unit is mAU, and the abscissa "Time" represents time, and the unit is min, that is,...

Embodiment 3

[0076] Embodiment 3: the detection method of the purity of 2-(2-chloro-1-ethylene) methyl hydrazide formate

[0077] 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 purity and impurity content of methyl 2-(2-chloro-1-ethylene)hydrazide formate in sample 3 to be tested were calculated by the area normalization method, and the results are shown in Table 3.

[0078] Figure 4 It is the chromatogram B obtained in the detection method of Example 3. Figure 4 "1" in represents the peak corresponding to methyl 2-(2-chloro-1-ethylene) hydrazide formate, Figure 4 "2" in represents the peak corresponding to "maximum simple heterogeneity" ( Figure 4 The ordinate "Absorbance" in the graph represents absorbance, and the unit is mAU, and the abscissa "Time" represents time, and the unit is min, that is, minutes).

[0079] table 3

[0080]

[0081] As can be seen from Table...

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Abstract

The invention belongs to the technical field of analysis, and discloses a method for detecting the purity of methyl 2-(2-chloro-1-ethylene) hydrazide formate. The detection method comprises the following steps: dissolving a2-(2-chloro-1-ethylene) chloromethyl formate 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; and taking the to-be-detected sample solution, detecting the to-be-detected sample solution by liquid chromatography, and recording a chromatogram B, calculating the purity according to the chromatogram A and the chromatogram B; wherein the conditions of the liquid chromatography comprise a mobile phase A and a mobile phase B, the mobile phase A is a phosphate buffer solution and acetonitrile, the mobile phase B is acetonitrile; wherein the volume ratio of the phosphate buffer solution to acetonitrile in the mobile phase A is (950+ / -8): (50+ / -0.8). The detection method can be used for accurately detecting the purity of the 2-(2-chloro-1 ethylene) hydrazide methyl formate in the sample to be detected.

Description

technical field [0001] The invention belongs to the technical field of analysis, in particular to a method for detecting the purity of methyl 2-(2-chloro-1-ethylene)hydrazide formate. Background technique [0002] Aprepitant, also known as aceminidazole, is a off-white to light yellow crystal-like solid chemical, which is mainly used clinically to prevent acute and delayed side effects during the initial and repeated treatment of highly emetogenic anticancer chemotherapy Sexual nausea and vomiting. 2-(2-Chloro-1-ethylene)hydrazide methyl formate, its CAS number is 155742-64-6, 2-(2-chloro-1-ethylene)hydrazide methyl formate is produced An important intermediate of prepitant, the purity and impurity content of methyl 2-(2-chloro-1-ethylene)hydrazide formate directly affect the purity and impurity content of aprepitant, thus directly affecting the purity of aprepitant. Drug efficacy of Pittan. [0003] In the process of preparing aprepitant, the detection of the purity and ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
Inventor 蒙发明陈舒婷罗凤玲胡骆祥
Owner ENANTIOTECH CORP
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