Sertraline hydrochloride intermediates (+/-)-tetralone and chiral chromatographic splitting method thereof

A technology of sertraline hydrochloride and chiral chromatography, which is applied in the directions of material separation, analysis materials, measuring devices, etc., can solve the problems such as infeasible chemical separation methods, and achieve the effect of quality control

Inactive Publication Date: 2014-10-29
RAFFLES PHAMRMATECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Since the (±)-Tetralone racemate molecule has no active groups such as hydroxyl, carboxyl or amino groups, chemical resolution is not feasible, only chromatographic resolution

Method used

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  • Sertraline hydrochloride intermediates (+/-)-tetralone and chiral chromatographic splitting method thereof
  • Sertraline hydrochloride intermediates (+/-)-tetralone and chiral chromatographic splitting method thereof
  • Sertraline hydrochloride intermediates (+/-)-tetralone and chiral chromatographic splitting method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Instruments and Conditions

[0039] High performance liquid chromatography: Shimadzu LC-15C

[0040] Chromatographic column: Enantiopak CCDP column (150x4.6 mm)

[0041] Mobile phase: n-hexane:isopropanol=95:5 (v:v)

[0042] Flow rate: 1.0mL / min

[0043] Injection volume: 10μL

[0044] Detection wavelength: 214nm (maximum absorption wavelength)

[0045] Experimental steps:

[0046] Weigh 25 mg of sertraline intermediate (±)-Tetralone, place it in a 25.00 mL volumetric flask, add mobile phase to dilute to 25.00 mL. as a mixed sample solution.

[0047] Take 4 respectively S - Tetralone and 4 R - Tetralone each 25mg, respectively placed in 25.00mL volumetric flask, adding mobile phase to dilute to 25.00mL, as a qualitative control solution.

[0048] Take the control solution and the mixed sample solution respectively, carry out high-performance liquid chromatography separation and analysis according to the above conditions, and record the chromatograms. see attac...

Embodiment 2

[0050] Instruments and Conditions

[0051] High performance liquid chromatography: Shimadzu LC-15C

[0052] Column: Enantiopak CADP column (150x4.6 mm)

[0053] Mobile phase: n-hexane: ethanol = 99:1 (v:v)

[0054] Flow rate: 1.0mL / min

[0055] Injection volume: 10μL

[0056] Detection wavelength: 214nm (maximum absorption wavelength)

[0057] Experimental steps:

[0058] Weigh 25mg of sertraline intermediate (±)-Tetralone, place it in a 25.00mL volumetric flask, add mobile phase to dilute to 25.00mL. as a mixed sample solution.

[0059] Take 4 respectively S - Tetralone and 4 R - Tetralone each 25mg, respectively placed in 25.00mL volumetric flask, adding mobile phase to dilute to 25.00mL, as a qualitative control solution.

[0060] Take the control solution and the mixed sample solution respectively, carry out high-performance liquid chromatography separation and analysis according to the above conditions, and record the chromatograms. see attached results figure...

Embodiment 3

[0062] Instruments and Conditions

[0063] High performance liquid chromatography: Shimadzu LC-15C

[0064] Chromatographic column: Enantiopak CCDP column (150x4.6 mm)

[0065] Mobile phase: n-hexane: ethanol = 90:10 (v:v)

[0066] Flow rate: 1.0mL / min

[0067] Injection volume: 10μL

[0068] Detection wavelength: 214nm (maximum absorption wavelength)

[0069] Experimental steps:

[0070] Weigh 25 mg of sertraline intermediate (±)-Tetralone, place it in a 25.00 mL volumetric flask, add mobile phase to dilute to 25.00 mL. as a mixed sample solution.

[0071] Take 4 respectively S - Tetralone and 4 R - Tetralone each 25mg, respectively placed in 25.00mL volumetric flask, adding mobile phase to dilute to 25.00mL, as a qualitative control solution.

[0072] Take the control solution and the mixed sample solution respectively, carry out high-performance liquid chromatography separation and analysis according to the above conditions, and record the chromatograms. see attac...

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Abstract

The invention relates to a liquid chromatographic separation and analysis method, and particularly relates to sertraline hydrochloride intermediates (+ / -)-tetralone and a chiral chromatographic splitting method thereof. The sertraline hydrochloride intermediates (+ / -)-tetralone and the chiral chromatographic splitting method thereof are provided, wherein the method comprises the following steps: taking the sertraline hydrochloride intermediates (+ / -)-tetralone, and dissolving in an aliphatic hydrocarbon-alcohol mixed liquid; and providing a polysaccharide chiral stationary phase, taking the solution for sample introduction, and carrying out chiral chromatographic separation under a condition with the aliphatic hydrocarbon-alcohol mixed liquid as a mobile phase. A coating type polysaccharide chiral stationary phase material is adopted for effective separation and analysis on the sertraline hydrochloride intermediates and enantiomers thereof, impurities brought by preparation of sertraline hydrochloride with a new process are effectively controlled, and the quality of raw material drugs and preparations can be further controlled.

Description

Technical field [0001] The invention involves the separation analysis method of hand-to-hand compounds, and specifically involves a method of splitting the intermediate (±) -Tetralone and its hand chromatographic splitting methods. Background technique [0002] Hydrochloride Hydrochloride (product name ZOLOFT, Zuo Luo Fu) is an anti -mental depression developed by Pfizer in the early 1990s. It has the advantages of long -term effects and few side effects.The medicine was first listed in the UK in December 1990. It was listed in the United States in 1992. It is currently listed in more than 13 countries. [0003] It has been reported that there are many ways to prepare Hydrochloride, but the previous industry mainly adopts the split method reported by Pfizer Company. The process is as shown below., 1984).α-与 phenol and neighbors are in Alcl 3 Under the catalytic, the reaction obtained 4- (3,4-dichlorophenyl) -1-ketone ((±) -tetralone).(±) -tetralone reacts with N-methyl hydroxylam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 安德鲁·菲利斯章伟光范军叶伟平孙家强
Owner RAFFLES PHAMRMATECH CO LTD
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