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Method for determining (4R, 6R) -6-aminoethyl-2,2-dimethyl-1,3-dioxane-4- tert-butyl acetate content

A dioxane and content technology, applied in the field of pharmaceutical and chemical quality testing, can solve the problems of no content measurement and reporting, and achieve a good linear relationship

Active Publication Date: 2015-12-09
HENAN ZHIWEI BIOMEDICINE CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis and detection of ATS-9 have been reported in many literatures, such as Junjie Liu et al. using (4R,6R)-6-azidoethyl-2,2-dimethyl-1,3-dioxane-4 -Methyl acetate is used as raw material, hydrolyzed under alkaline conditions, and then esterified with di-tert-butyl dicarbonate, and finally the product ATS-9 is generated under the catalysis of triphenylphosphine (JunjieLiu, Che-ChangHsu, Chi-HueyWong.TetrahedronLetters, 45 , 2439-2441); Fang-JunXiong et al. used (R)-2-chloro-ethylene oxide as the starting material, and finally synthesized ATS-9 through multi-step reactions (Fang-JunXiong, JieLi, Xiao-FeiChen, Wen- XueChen, Fen-ErChen.Tetrahedron: Asymmetry, 25, 1205-1208); YujiKawato et al. used (R)-5-benzyl-3-hydroxy-N,N-dialkylpentanethioamide as raw material, after many ATS-9 was synthesized by step reaction (YujiKawato, MitsutakaIwata, RyoYazaki, NaoyaKumagai, MasakatsuShibasaki.Tetrahedron, 67, 6539-6546); Blackley performed GC-MS on ATS-9 with FactorFourVF-5MS (30m*0.25mm) capillary column Detection (Blackley, US8563753B2, 2013.10.22), but there is no report on its content determination

Method used

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  • Method for determining (4R, 6R) -6-aminoethyl-2,2-dimethyl-1,3-dioxane-4- tert-butyl acetate content
  • Method for determining (4R, 6R) -6-aminoethyl-2,2-dimethyl-1,3-dioxane-4- tert-butyl acetate content
  • Method for determining (4R, 6R) -6-aminoethyl-2,2-dimethyl-1,3-dioxane-4- tert-butyl acetate content

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Experimental program
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Effect test

Embodiment 1

[0029] ThermoFisher TG-624 capillary gas chromatographic column (30m*0.32mm, 1.8μm) was used; the column temperature was kept at 150°C for 2 minutes, the temperature was raised to 220°C at a heating rate of 40°C / min and kept for 3 minutes, and the temperature was raised to 20°C / min at a heating rate of 20°C / min. Keep at 240°C for 8 minutes; vaporization chamber temperature 300°C; column flow rate 2.5mL / min, split ratio 30:1; detector is hydrogen flame ionization detector, temperature 300°C; carrier gas is high-purity nitrogen; 2μL; air flow 400mL / min, hydrogen flow 35mL / min, make-up gas flow 40mL / min. Accurately weigh an appropriate amount of ATS-9 test product (batch number 20141012) into a 10mL volumetric flask, dilute with ethyl acetate to make a stock solution of the test product with a mass concentration of about 20mg / mL; accurately pipette 0.8mL of the above The test product stock solution was placed in a 5mL volumetric flask, diluted with ethyl acetate to a constant vol...

Embodiment 2

[0031] AgilentDB-624 capillary gas chromatographic column (30m*0.32mm, 1.8μm) is used, the column temperature is 240°C for 20min; the vaporization chamber temperature is 250°C; the column flow rate is 1.0mL / min, the split ratio is 20:1; the detector is hydrogen flame ion The temperature is 270°C; the carrier gas is high-purity nitrogen; the injection volume is 2 μL; the air flow rate is 400 mL / min, the hydrogen flow rate is 35 mL / min, and the makeup gas flow rate is 40 mL / min. Accurately weigh the ATS-9 test product (batch number 20141101) in a 10mL volumetric flask, dilute with 1,2-dichloroethane to make a stock solution of the test product with a mass concentration of about 20mg / mL; precision Pipette 0.8mL of the above-mentioned stock solution of the test product into a 5mL volumetric flask, dilute with 1,2-dichloroethane to a constant volume and shake well to obtain the test solution. Take the above-mentioned test solution and inject it into a gas chromatograph, and measure...

Embodiment 3

[0033] Using ThermoFisher TG-5MS capillary gas chromatography column (30m*0.32mm, 0.5μm), the column temperature is 100°C for 3 minutes, and the temperature is raised to 320°C at a heating rate of 10°C / min for 20 minutes; the vaporization chamber temperature is 300°C; the column flow rate is 2.5mL / min, split ratio 30:1; the detector is a hydrogen flame ionization detector, the temperature is 320°C; the carrier gas is high-purity nitrogen; the air flow rate is 400mL / min, the hydrogen flow rate is 35mL / min, and the makeup gas flow rate is 40mL / min ; The injection volume was 2.5 μL. Accurately weigh the ATS-9 test product (batch number 20141205) and place it in a 10mL volumetric flask, dilute it with DMF to make a stock solution of the test product with a mass concentration of about 20mg / mL; pipette the stock solution of the test product accurately 1.0mL was placed in a 5mL volumetric flask, diluted with DMF and shaken to obtain the test solution. Get above-mentioned need testi...

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Abstract

The present invention discloses a method for determining (4R, 6R) -6--aminoethyl-2,2-dimethyl-1,3-dioxane-4- tert-butyl acetate content. The method is as follows: ATS-9 is diluted with 1,2-dichloroethane, an Agilent DB-624 capillary gas chromatography column is used, a hydrogen flame ionization detector is used, appropriate temperature programing, vaporization chamber temperature and detector temperature are set, nitrogen is used as a carrier gas, n-hexadecane is used as an internal standard for detection, and ATS-9 content in a to-be-tested solution can be calculated by internal standard method according to the gas chromatogram. The ATS-9 and related substances and the internal standard can be effectively separated, and the method is rapid, accurate, simple and well reproducible, and lays the foundation for the establishment of ATS-9 quality standards.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical and chemical quality detection, and specifically relates to a method for determining (4R,6R)-6-aminoethyl-2,2-dimethyl-1,3-dioxane-4-tert-butyl acetate content method. Background technique [0002] (4R,6R)-6-aminoethyl-2,2-dimethyl-1,3-dioxane-4-tert-butyl acetate, abbreviated as ATS-9, the molecular formula is C 14 h 27 NO 4 , the English name is (4R, cis)-1,1-Dimethylethyl-6-aminoethyl-2,2-dimethyl-1,3-dioxane-4-acetate, and its chemical structure is , is a key intermediate in the synthesis of atorvastatin calcium. The trade name of atorvastatin calcium is Lipitor, which belongs to statin drugs and is an effective drug for the treatment of hypercholesterolemia and mixed hyperlipidemia. Company) developed by the company, and was approved by the FDA to be marketed in the United States in 1997, and its patent protection expired in 2011. [0003] As a key intermediate for the synthesis...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 徐桂清贾淑红姜玉钦张玮玮毛龙飞董文佩申家轩蒋涛李伟
Owner HENAN ZHIWEI BIOMEDICINE CO LTD
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