Analysis method for bisindole compound optical isomer

A technology for optical isomers and analysis methods, applied in the field of separating two bisindole compounds by high performance liquid chromatography, can solve problems such as difficult separation, and achieve the effect of simple operation

Active Publication Date: 2013-11-06
枣庄市新星钢结构有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the two compounds are basic, it is difficult to split the diamines (Yang Huilai, Synthesis and Resolution Research of Binaphthol,

Method used

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  • Analysis method for bisindole compound optical isomer
  • Analysis method for bisindole compound optical isomer
  • Analysis method for bisindole compound optical isomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Instruments and Conditions

[0031] High performance liquid chromatograph: Shimadzu LC-20A;

[0032] Chromatographic column: Chiralcel AD-H (Daicel, 250mm×4.6mm, 5μm) silica gel surface coated with cellulose-tris(3,5-xylylcarbamate) chiral column;

[0033] Mobile phase volume ratio: the volume ratio of n-hexane and isopropanol is 70:30;

[0034] Detection wavelength: 254nm;

[0035] Flow rate: 1.0mL / min;

[0036] Injection volume: 10 μL;

[0037] Column temperature: 25°C.

[0038] Experimental procedure: Take 5 mg of 4b,9b-diphenyl-4b,5,9b,10-tetrahydroindole[3,2-b]indole sample and put it in a 10mL volumetric flask, add isopropanol to dissolve and dilute to Scale, shake well, and filter through a filter membrane as a sample solution. The sample solution was taken and analyzed by high performance liquid chromatography under the above conditions, and the chromatogram was recorded.

[0039] The results are attached figure 1 , it can be seen that under this conditi...

Embodiment 2

[0041] Instruments and Conditions

[0042] High performance liquid chromatograph: Shimadzu LC-20A;

[0043] Chromatographic column: Chiralcel IA (Daicel, 250mm×4.6mm, 5μm) silica gel surface bonded with cellulose-tris(3,5-xylylcarbamate) chiral column;

[0044] Mobile phase volume ratio: the volume ratio of n-hexane and isopropanol is 95:5;

[0045] Detection wavelength: 254nm;

[0046] Flow rate: 1.0mL / min;

[0047] Injection volume: 10 μL;

[0048] Column temperature: 25°C.

[0049] Experimental steps:

[0050] Take 5 mg of 4b,9b-diphenyl-4b,5,9b,10-tetrahydroindole[3,2-b]indole sample into a 10mL volumetric flask, add isopropanol to dissolve and dilute to the mark, shake Homogeneous, filtered with a filter membrane, as the sample solution. The sample solution was taken and analyzed by high performance liquid chromatography under the above conditions, and the chromatogram was recorded.

[0051] The results are attached figure 2 , it can be seen that under this cond...

Embodiment 3

[0053] Instruments and Conditions

[0054] High performance liquid chromatograph: Shimadzu LC-20A;

[0055]Chromatographic column: Chiralcel OD-H (Daicel, 250mm×4.6mm, 5μm) silica gel surface coated with amylose-tris(3,5-xylylcarbamate) chiral column;

[0056] Mobile phase volume ratio: the volume ratio of n-hexane and isopropanol is 90:10;

[0057] Detection wavelength: 254nm;

[0058] Flow rate: 1.0mL / min;

[0059] Injection volume: 10 μL;

[0060] Column temperature: 25°C.

[0061] Experimental steps:

[0062] Take 5 mg of 3,8-dichloro-4b,9b-diphenyl-4b,5,9b,10-tetrahydroindole[3,2-b]indole sample into a 10mL volumetric flask, add isopropanol Dissolve and dilute to volume, shake well, filter through filter membrane, and use as sample solution. The sample solution was taken and analyzed by high performance liquid chromatography under the above conditions, and the chromatogram was recorded.

[0063] The results are attached image 3 , it can be seen that under this c...

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Abstract

The invention aims to provide a high performance liquid chromatography method for analysis of a tetrahydroindole compound and realizes chiral analysis determination of the tetrahydroindole compound for the first time. According to a technical scheme adopted by the invention, the method for analysis of a bisindole compound optical isomer is characterized in that: the analysis method is high performance liquid chromatography, amylose or a cellulose derivative is taken as a stationary phase chiral chromatographic column, a normal phase solvent is adopted as a mobile phase, the detection wavelength is 254nm, and the analysis is carried out at room temperature. By employing different types of chiral columns to separate two bisindole compounds, the method provided in the invention has the advantages of simple and rapid operation. And a method for separation of medicine and pesticide intermediates is provided.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography, in particular to a method for separating two bisindole compounds by using high-performance liquid chromatography. Background technique [0002] 4b,9b-diphenyl-4b,5,9b,10-tetrahydroindole[3,2-b]indole and 3,8-dichloro-4b,9b-diphenyl-4b,5,9b ,10-Tetrahydroindole[3,2-b]indole Two tetrahydroindole compounds composed of 6,12-diphenyldibenzo[b,f][1,5]diazepine Tetraene and 3,9-dichloro-6,12-diphenyldibenzo[b,f][1,5]diazacyclooctatetraene were obtained by reduction with specific solvents (W.Metlesics, R. Tavares, L.H. Sternbach, J. Org. Chem. 1966, 31, 3356). Although the two compounds are basic, it is difficult to resolve diamines like (Yang Huilai, Synthesis and resolution of binaphthol, binaphthylamine, and binaphtholamine, Zhejiang, Zhejiang University of Technology, 2006) to obtain chiral isomers. In view of the unique and efficient physiological activity of tetrahydroindole compounds...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 孙小强靳琳琳李正义钱纪生陈亮
Owner 枣庄市新星钢结构有限公司
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