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A kind of detection method of aprepitant intermediate

A detection method, the technology of aprepitant, 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: 2021-06-01
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of detection method of aprepitant intermediate
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  • A kind of detection method of aprepitant intermediate

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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 Peak time (min) Peak area ratio (%) main peak resolution Main peak theoretical plate number APT07 6.670 99.30％ 2.37 9034 toluene 5.460 0.17％ / / To remove fluorine impurities 7.337 0.12％ / / APT04 / / / / N-Bn impurity / / / / maximum complex 3.033 0.16％ / / total miscellaneous / 0.70％ / /

[0063] Table 3 Test results of test product 3

[0064] Impurities Peak time (min) Peak area ...

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Abstract

The invention discloses a detection method for an aprepitant intermediate, which is detected by a liquid chromatograph, and quantitatively analyzed by an area normalization method, and the chromatographic conditions are as follows: chromatographic column: C18 chromatographic column, injection volume: 15- 25μl, flow rate: 0.8‑1.2ml / min, column temperature: 25‑35°C, detection wavelength: 210‑220nm, mobile phase: mobile phase A: 0.1‑0.3% potassium dihydrogen phosphate solution, pH7.0; mobile phase B: acetonitrile; the volume ratio of mobile phase A and mobile phase B is (15-25): (75-85), diluent: acetonitrile, detector: ultraviolet detector; detection method of the present invention is simple, fast, can realize p-(2R,3S)‑2‑[(1R)‑1‑[3,5‑bis(trifluoromethyl)phenyl]ethoxy]‑3‑(4‑fluorophenyl)‑morpholine hydrochloride Accurate determination of salt with high sensitivity.

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 Patents(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