Method for detecting aprepitant intermediate

A detection method and aprepitant technology, applied in the field of analytical chemistry, can solve problems such as undiscovered, and achieve the effect of simple operation and high sensitivity

Active Publication Date: 2018-05-04
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, no (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3-(4-fluorophenyl)- Related documents and reports on the purity detection method of morpholine hydrochloride, in order to strengthen (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy ]-3-(4-fluorophenyl)-morpholine hydrochloride quality control needs to develop its detection method

Method used

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  • Method for detecting aprepitant intermediate
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  • Method for detecting aprepitant intermediate

Examples

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Embodiment 1

[0039] A prepitant intermediate (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3-(4-fluorobenzene base)-morpholine hydrochloride detection method

[0040] 1. Instruments and testing conditions

[0041] Shimadzu LC-15C high performance liquid chromatography, the chromatographic column is WondaSil C18Superb (4.6*250mm, 5um);

[0042] Injection volume: 20μl;

[0043] Flow rate: 1ml / min;

[0044] Column temperature: 30°C;

[0045] Detection wavelength: 215nm;

[0046] Mobile phase: The volume ratio of mobile phase A to mobile phase B is 20:80; among them, mobile phase A is to take 1.36g of potassium dihydrogen phosphate and dissolve it in 1L of water, and adjust the pH to 7.0 with saturated sodium hydroxide solution; mobile phase B is acetonitrile;

[0047] Diluent: acetonitrile;

[0048] Detector: UV detector;

[0049]Quantitative method: area normalization method;

[0050] 2. Experimental steps

[0051] Adopt high-performance liquid chromatography to detect,...

Embodiment 2

[0057] Take three batches of (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3-(4-fluoro Phenyl)-morpholine hydrochloride product, respectively test sample 1-3, detects according to the detection method of embodiment 1, adopts area normalization method to carry out purity and impurity calculation thereof, and test result sees the following table 1- 3:

[0058] Table 1 Test results of test product 1

[0059]

[0060]

[0061] Table 2 Test results of test product 2

[0062] Impurities

[0063] Table 3 Test results of test product 3

[0064] Impurities

[0065] The detection method of the present invention can detect (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy group easily, accurately, quickly, efficiently and reliably The purity and impurity content of ]-3-(4-fluorophenyl)-morpholine hydrochloride have high sensitivity, and are easy to operate and can be completely separated, thereby providing research and development and quali...

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Abstract

The invention discloses a method for detecting an aprepitant intermediate. According to the method, a liquid chromatograph is adopted for detection, quantitative analysis is implemented by using an area normalization method, and spectrum conditions are as follows: a C18 spectrum column is adopted as a spectrum column; the feeding amount is 15-25mu l; the flowing speed is 0.8-1.2ml/minute; the column temperature is 25-35 DEG C; the detection wavelength is 210-220nm; the mobile phase includes a mobile phase 0.1-0.3% monopotassium phosphate solution of which the pH value is 7.0, and a mobile phase B acetonitrile; the volume ratio of the mobile phase A to the mobile phase B is (15-25):(75-85); acetonitrile is adopted as a dilution liquid; and a ultraviolet detector is adopted as a detector. The method disclosed by the invention is simple and rapid, accurate testing on (2R,3S)-2-[(1R)-1-[3,5-bi(trifluoromethyl) phenyl] ethyoxyl]-3-(4-fluorophenyl) morpholine hydrochloride is achieved, and very high sensitivity is achieved.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a detection method of an aprepitant intermediate. Background technique [0002] Aprepitant, whose chemical name is 5-[2(R)-[1(R)-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3(S)-(4 -Fluorophenyl)morpholin-4-ylmethyl]-3,4-dihydro-2H-1,2,4-triazol-3-one; Aprepitant; 5-(2(R)- (1(R)-(3,5-bis(trifluoromethyl)phenyl)ethoxy)-3(S)-(4-fluorophenyl)morpholin-4-ylmethyl)-3, 4-Dihydro-2H-1,2,4-triazol-3-one for the treatment of depression and chemotherapy-induced emesis. It can prevent acute and delayed nausea and vomiting caused by the first and subsequent repeated chemotherapy. [0003] (2R,3S)-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3-(4-fluorophenyl)-morpholine hydrochloride , its CAS number is 171482-05-6, and its structural formula is as follows. It is an important intermediate for the production of aprepitant, and its purity and impurities will direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 蒙发明曹欢燕徐亮邓超芹俞伟文樊志麒
Owner ENANTIOTECH CORP
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