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Aprepitant intermediate detection method

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

Inactive Publication Date: 2018-04-10
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no chirality of (2R)-4-benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]morpholin-3-one In order to strengthen the relevant literature and reports on the purity detection method of (2R)-4-benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]? The quality control of lin-3-one needs to develop (2R)-4-benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]morpholine The detection method of -3-ketone, especially the detection method of its chiral purity

Method used

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Embodiment 1

[0041] A detection method for (2R)-4-benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]morpholin-3-one

[0042] 1. Instruments and testing conditions

[0043] Shimadzu LC-15C high performance liquid chromatography, the chromatographic column is chiralcel OD-H, the specification of the chromatographic column is 4.6*250mm, 5μm. That is, the filler particle size of the chromatographic column is 5 μm, the pore diameter is 4.6 mm, and the column length of the chromatographic column is 250 mm. Flow rate: 0.8ml / min; Column temperature: 25°C; Detection wavelength: 215nm; Detector: UV detector, injection volume: 20μl.

[0044] Mobile phase: n-hexane: isopropanol, the volume ratio is 980:20;

[0045] Diluent: n-hexane: isopropanol, the volume ratio is 50:50.

[0046] 2. Experimental steps

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Abstract

The invention discloses an aprepitant intermediate detection method. An aprepitant intermediate is (2R)-4-benzyl-2-[(1R)-1-[3,5,bis(trifluoromethyl)phenyl]ethoxy]morpholine-3-ketone. The detection method comprises the steps that detection is conducted through a high performance liquid chromatograph, and quantitative analysis is conducted through an area normalization method; the chromatographic conditions are that a chromatographic column is chiralcel OD-H, the sample size ranges from 15 microliters to 25 microliters, the flow velocity ranges from 0.7 ml / min to 0.9 ml / min, the column temperature ranges from 10 DEG C to 40 DEG C, the detection wavelength ranges from 212 nm to 218 nm, the mobile phase is prepared from n-hexane and isopropanol, the volume ratio of n-hexane to isopropanol is (40-60):50, and a detector is an ultraviolet detector. By means of the detection method, rapid and accurate determination on (2R)-4-benzyl-2-[(1R)-1-[3,5,bis(trifluoromethyl)phenyl]ethoxy]morpholine-3-ketone can be achieved, the sensitivity is very high, operation is easy, complete separation can be achieved, and the basis of research and development and quality detection can be provided for researching the compound.

Description

technical field [0001] The invention relates to a detection method for an aprepitant intermediate, belonging to the technical field of drug analysis, in particular to (2R)-4-benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl) ) Detection method of phenyl] ethoxy] morpholin-3-one. Background technique [0002] (2R)-4-Benzyl-2-[(1R)-1-[3,5-bis(trifluoromethyl)phenyl]ethoxy]morpholin-3-one, whose CAS number is 287930- 75-0 is an important intermediate for the production of Aprepitant, and its chiral purity and isomer impurities directly affect the chiral purity of Aprepitant and the amount of isomer impurities, thus directly affecting the quality of Aprepitant. Efficacy of pitan drugs. [0003] Aprepitant, also known as aceminidazole, is mainly used to prevent acute and delayed nausea and vomiting during the initial and repeated treatment of highly emetogenic anticancer chemotherapy, and its chemical name is 5-[2(R )-[1(R)-[3,5-bis(trifluoromethyl)phenyl]ethoxy]-3(S)-(4-fluorophenyl)...

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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