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Method for separating and detecting related substances of 1-butylsulfonyl chloride

A technology for butylsulfonyl chloride and related substances, which is applied in the field of separation and detection of 1-butylsulfonyl chloride related substances, and achieves the effects of rapid derivatization reaction, less corrosion and less reaction by-products

Pending Publication Date: 2021-06-04
SICHUAN KELUN PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There is no relevant report on the separation and detection of 1-butylsulfonyl chloride related substances in the prior art, so it is necessary to develop a separation and detection method of 1-butylsulfonyl chloride related substances

Method used

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  • Method for separating and detecting related substances of 1-butylsulfonyl chloride
  • Method for separating and detecting related substances of 1-butylsulfonyl chloride
  • Method for separating and detecting related substances of 1-butylsulfonyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] S1: Sample preparation:

[0045] 1. Preparation of the test solution: Take about 125mg of 1-butylsulfonyl chloride test product, weigh it accurately, add 3ml of dichloromethane, shake well, add 0.4ml of diethylamine, vortex for 1min, add dichloromethane Dissolve and dilute to 25ml. Accurately measure 10ml, add 5ml of water, shake for 1min, take 10ml of the organic layer, add an appropriate amount of anhydrous sodium sulfate (about 1g), remove water, and take the supernatant as the test solution.

[0046] 2. Blank solution: do not add the 1-butylsulfonyl chloride test product, and prepare a blank solution according to the preparation method of the test product solution.

[0047] 3. System suitability solution:

[0048] 1-Butylsulfonyl chloride derivative stock solution, ethylsulfonyl chloride derivative stock solution, propylsulfonyl chloride derivative stock solution, pentanesulfonyl chloride derivative stock solution, hexylsulfonyl chloride derivative stock solution:...

Embodiment 2

[0065] 2.1 Specificity

[0066] Measure 1 μl of the system suitability solution, blank solution and test solution respectively, and inject them into the gas chromatograph for detection. The gas chromatogram is as follows: Figure 1~3 shown by the spectrum Figure 1~3 It can be seen that the blank solution does not interfere with the determination of 1-butylsulfonyl chloride and various impurities, and the resolution between 1-butylsulfonyl chloride and various impurities is greater than 2.0, which is good and meets the requirements.

[0067] 2.2 Linear range and correction factor, detection limit and quantification limit

[0068] Take 1-butylsulfonyl chloride derivative stock solution, ethylsulfonyl chloride derivative stock solution, propylsulfonyl chloride derivative stock solution, pentanesulfonyl chloride derivative stock solution, hexylsulfonyl chloride derivative stock solution, 1,2 -Dichloroethane stock solution, 1-bromobutane stock solution, and butyl thiocyanate sto...

Embodiment 3

[0082] Chromatographic conditions:

[0083] Chromatograph: Agilent 7890B

[0084] Detector: Hydrogen Flame Ionization Detector (FID)

[0085] Chromatographic column: HP-5 capillary column (30m×0.320mm×0.25μm);

[0086] Injection port temperature: 210°C;

[0087] Detector temperature: 240°C;

[0088] Carrier gas flow rate: 1.8ml / min;

[0089] Split ratio: 4:1;

[0090] Injection volume: 1μl;

[0091] Programmable temperature rise: the initial temperature is 33°C, maintained for 2 minutes, then raised to 215°C at a rate of 18°C / min, maintained for 7 minutes.

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Abstract

The invention provides a method for separating and detecting related substances of 1-butylsulfonyl chloride, which comprises the following steps: dissolving 1-butylsulfonyl chloride in a solvent to prepare a solution, adding an amine reagent into the solution for reaction, and detecting and analyzing by adopting GC. According to the method, all impurities and main components are effectively separated, the specificity, sensitivity, accuracy, precision and the like of the method meet the requirements, and the method can be used for separating and detecting related substances of 1-butylsulfonyl chloride.

Description

technical field [0001] The invention relates to a method for analyzing related substances of 1-butylsulfonyl chloride, in particular to a method for separating and detecting related substances of 1-butylsulfonyl chloride. Background technique [0002] 1-Butylsulfonyl chloride is a common sulfonating agent for the synthesis of pharmaceutical intermediates, active ingredients and other specialty chemicals. The production of 1-butylsulfonyl chloride produces impurities that vary by different manufacturers and chemical processes. The homologue impurities or other active impurities it may contain may also become impurities in the active pharmaceutical ingredient (API) through the alkylation reaction. Therefore, in order to control the quality of raw materials, a sensitive and accurate method is needed to detect the content of related substances in 1-butylsulfonyl chloride. [0003] In general, sulfonyl chlorides have high reactivity in the presence of water and form sulfonic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/067G01N2030/062G01N2030/8845
Inventor 孙鹏张小林杨敏林保全韩庆平赵忠琼王晶翼
Owner SICHUAN KELUN PHARMA RES INST CO LTD
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