Normal-phase chromatography analysis method for 4-chloro-2-nitrophenyl isocyanate and reaction liquid thereof

A technology of nitrophenyl isocyanate and normal phase chromatography, which is applied in the field of normal phase chromatography analysis, can solve the problem that 4-chloro-2 nitrophenyl isocyanate cannot be analyzed at the same time, and achieve the effect of rapid method and good repeatability

Active Publication Date: 2019-07-30
LIANHE CHEM TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The technical problem to be solved by the present invention is to overcome the need for prior derivatization and the inability to simultaneo...

Method used

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  • Normal-phase chromatography analysis method for 4-chloro-2-nitrophenyl isocyanate and reaction liquid thereof
  • Normal-phase chromatography analysis method for 4-chloro-2-nitrophenyl isocyanate and reaction liquid thereof
  • Normal-phase chromatography analysis method for 4-chloro-2-nitrophenyl isocyanate and reaction liquid thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Direct quantitative analysis of 4-chloro-2-nitrophenyl isocyanate

[0044] 1. Chromatographic separation and detection conditions

[0045] Chromatographic column: Agilent's normal-phase silica gel column RX-SIL (diameter and length: 4.6×100 mm, silica gel particle diameter: 1.8 μm).

[0046] Mobile phase: 0.10% trifluoroacetic acid ~ 99.90% n-hexane, total water content <0.01%.

[0047] Flow rate: 1.0ml / min

[0048] Column temperature: 25°C

[0049] Detection wavelength of UV detector: 230nm

[0050] Injection volume: 1.0μL

[0051] 2. Preparation of standard solution and sample solution

[0052] Accurately weigh 30mg, 60mg, 90mg, 120mg and 150mg (accurate to 0.0001g) of self-made standard samples of 4-chloro-2-nitrophenylisocyanate into a 10ml brown volumetric flask, add 0.10 % trifluoroacetic acid ~ 99.90% n-hexane dissolved and constant volume to obtain standard samples 1 ~ 5.

[0053]Accurately weigh a sample of 100 mg (accurate to 0.0001 g) of 4-chloro-2-nit...

Embodiment 2

[0067] The Intermediate Control Analysis of the Reaction Solution Synthesized from 4-Chloro-2-Nitroaniline and Phosgene at Normal Temperature

[0068] Chromatographic separation and detection conditions are the same as in Example 1.

[0069] Accurately weigh 0.02g (accurate to 0.0001g) of 4-chloro-2nitroaniline into a 25ml brown volumetric flask, add 0.10% trifluoroacetic acid-99.90% n-hexane with a total water content of image 3 .

[0070] Accurately pipette 0.2 g of the reaction solution into a 25 ml brown volumetric flask, add 0.10% trifluoroacetic acid-99.90% n-hexane with a total water content of <0.01% to dissolve and dilute to volume; obtain the sample to be analyzed.

[0071] The chromatographic analysis chart of the reaction solution under normal temperature conditions is shown in Figure 4 .

[0072] Under selected chromatographic conditions, using the above-mentioned analysis method, the external standard method can qualitatively determine whether there are raw m...

Embodiment 3

[0074] The intermediate control analysis of the reaction liquid synthesized from 4-chloro-2-nitroaniline and phosgene at 50℃ for the synthesis of 4-chloro-2-nitrophenyl isocyanate.

[0075] Chromatographic separation and detection conditions are the same as in Example 1.

[0076] Sampling analysis of the reaction solution sample configured in Example 2, the chromatographic analysis spectrum of the reaction solution at 50°C is shown in Figure 5 .

[0077] Under the selected chromatographic conditions, using the above analysis method, the external standard method can qualitatively determine whether there are raw materials, intermediate products and products in the reaction solution at 50°C. By using the area normalization method to relative quantify the by-products, when the main product 4-chloro-2-nitrophenyl isocyanate has the highest area percentage content, the optimal synthesis reaction conditions at 50°C are determined accordingly.

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Abstract

The invention discloses a normal-phase chromatography analysis method for 4-chloro-2-nitrophenyl isocyanate and reaction liquid thereof. A normal-phase silica gel column is used as a chromatographic column, an n-hexane-trifluoroacetic acid system is used as a mobile phase and a dissolvent, and an ultraviolet detector is adopted for detection. The method can be directly applied to quantitative analysis of the 4-chloro-2-nitrophenyl isocyanate, can also be used for intermediate control analysis of the reaction liquid synthesized with 4-chloro-2-nitroaniline and phosgene as raw materials, is rapid, accurate and good in repeatability, and can be used for detecting content changing conditions of raw materials, intermediate products and products in the reaction process and determining process conditions.

Description

technical field [0001] The invention relates to a normal phase chromatographic analysis method of 4-chloro-2 nitrophenyl isocyanate and its reaction solution. Background technique [0002] At present, the synthesis of 4-chloro-2-nitrophenyl isocyanate is mainly composed of 4-chloro-2-nitroaniline and phosgene as raw materials to generate 4-chloro-2-nitroanilide chloride, and then 4-chloro-2-nitroanilide -2-Nitroanilide chloride is further obtained by reflux reaction, the main reaction formula is formula 1: [0003] [0004] Formula 1 [0005] Wherein, because 4-chloro-2-nitrophenyl isocyanate and 4-chloro-2-nitrophenyl chloride are very sensitive to water, alcohol, amine and other substances, they cannot be directly analyzed and measured by reversed-phase liquid chromatography, nor can they Detect and analyze the intermediate product of 4-chloro-2-nitroanilide chloride generated by its reaction, so a method for directly, accurately and rapidly analyzing 4-chloro-2-nitro...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74Y02A50/30
Inventor 沈启富喻谨崔俊宁杨莲莲
Owner LIANHE CHEM TECH
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