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Method for determining four main components in N-isopropyl-anthranilamide synthetic reaction liquid

A technology of anthranilamide and anthranilic acid, which is applied in the field of determination of four main components in N-isopropyl-anthraniline synthesis reaction solution, achieves high accuracy and recovery rate, reduces drag Tail or forward tilt, guaranteed accuracy and repeatability

Pending Publication Date: 2022-06-28
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no existing technology for the simultaneous determination of isatoic anhydride, phthalimide, anthranilic acid, N-isopropyl-anthranilic acid amide

Method used

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  • Method for determining four main components in N-isopropyl-anthranilamide synthetic reaction liquid
  • Method for determining four main components in N-isopropyl-anthranilamide synthetic reaction liquid
  • Method for determining four main components in N-isopropyl-anthranilamide synthetic reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 (preferred conditions)

[0035] (1) Preparation of standard solution: Weigh 10.35mg isatoic anhydride, 10.46mg phthalimide, 9.91mg anthranilic acid, 25.03mg N-isopropyl-anthraniamide, and place them in the same 100ml In the volumetric flask, add acetonitrile ultrasonically to dissolve and dilute to the mark, and filter to obtain the mixed standard solution of each component.

[0036] (2) Preparation of sample solution: Accurately weigh 0.2513g of sample, add acetonitrile ultrasonically to dissolve and dilute to the mark, filter to obtain sample solution.

[0037] (3) Chromatographic conditions:

[0038] Using Shimadzu LC 2030C high performance liquid chromatograph, Inert Sustain C18 (250mm×4.6mm, 5μm) chromatographic column;

[0039] Flow rate: 0.8 mL / min;

[0040] Detector: diode array detector;

[0041] Detection wavelength: 239 nm;

[0042] Column temperature: 35℃;

[0043] Injection volume: 10 μL;

[0044] Mobile phase: mobile phase A is an aqueous ...

Embodiment 2

[0049](1) Preparation of standard solution: Weigh 5.13 mg of isatoic anhydride, 5.23 mg of phthalimide, 5.21 mg of anthranilic acid, and 15.03 mg of N-isopropyl-anthranilamide, and place them in the same In a 100mL volumetric flask, add acetonitrile to ultrasonic to dissolve and dilute to the mark, and filter to obtain a mixed standard solution of each component.

[0050] (2) Preparation of sample solution: Accurately weigh 0.1523g of the sample, add acetonitrile ultrasonically to dissolve and dilute to the mark, and filter to obtain the sample solution.

[0051] (3) Chromatographic conditions:

[0052] Using Shimadzu LC 2030C high performance liquid chromatograph, Thermo Hypersil GOLD C18 (250mm×4.6mm, 5μm) chromatographic column; flow rate: 0.6 mL / min;

[0053] Detector: diode array detector;

[0054] Detection wavelength: 244nm;

[0055] Column temperature: 35℃;

[0056] Column temperature: 20℃;

[0057] Injection volume: 5μL;

[0058] Mobile phase: mobile phase A is ...

Embodiment 3

[0063] (1) Prepare standard solution: Weigh 8.23mg isatoic anhydride, 7.20mg phthalimide, 8.21mg

[0064] Anthranilic acid and 30.03mg N-isopropyl-anthraniamide were placed in the same 100mL volumetric flask, acetonitrile was added to ultrasonically dissolve and diluted to the mark, and filtered to obtain a mixed standard solution of each component.

[0065] (2) Preparation of sample solution: Accurately weigh 0.3533g of the sample, add acetonitrile ultrasonically to dissolve and dilute to the mark, and filter to obtain the sample solution.

[0066] (3) Chromatographic conditions:

[0067] Using Shimadzu LC 2030C high performance liquid chromatograph, XBridge C18 (250mm×4.6mm, 5μm) chromatographic column;

[0068] Flow rate: 1.0 mL / min;

[0069] Detector: diode array detector;

[0070] Detection wavelength: 234 nm;

[0071] Column temperature: 40℃;

[0072] Injection volume: 20μL;

[0073] Mobile phase: mobile phase A is an aqueous solution adjusted with phosphoric acid ...

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Abstract

The invention discloses a method for determining four main components in a synthetic reaction solution of N-isopropyl-anthranilamide. According to the method, a C18 chromatographic column subjected to end capping treatment is adopted for separation, an ultraviolet detector or a diode array detector is adopted for detection, and the contents of phthalimide, isatoic anhydride, anthranilic acid and N-isopropyl-anthranilamide in an N-isopropyl-anthranilamide synthesis reaction solution are determined by a single-point external standard method. And a determination method is provided for central control analysis and reaction endpoint judgment of an N-isopropyl-anthranilamide synthesis process.

Description

technical field [0001] The invention relates to a method for simultaneous analysis and detection of isatoic anhydride, phthalimide, anthranilic acid and N-isopropyl-anthranilamide in the production process of N-isopropyl-anthranilamide . Background technique [0002] N-Isopropyl-Anthranilamide is an important intermediate in the synthesis of the herbicide bendazon, and can also be used as a raw material for the synthesis of pharmaceutical intermediates. The synthesis method of N-isopropyl-anthranilamide is based on isatoic anhydride and phthalimide as raw materials, oxidized with strong oxidant and then reacted with isopropylamine to prepare. The main components in the reaction solution are raw material isatoic anhydride, phthalimide, product N-isopropyl-anthraniline and by-product anthranilic acid. Because the impurity anthranilic acid exists in the intermediate N-isopropyl-anthranilamide and the final product bendazone, the quality of bendazone is unstable, and long-term...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065
Inventor 邢伶王瑞菲王艳刘友彬张晓霞岳涛
Owner QINGDAO UNIV OF SCI & TECH
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