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Detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide

A detection method, the technology of benzenesulfonamide, is applied in the field of analytical chemistry to achieve the effects of improved peak shape, high sensitivity, and easy operation

Active Publication Date: 2018-05-15
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are no relevant literature and reports on the purity detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzenesulfonamide. -4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzenesulfonamide quality control needs to develop its detection method

Method used

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  • Detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide
  • Detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide
  • Detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide

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Embodiment 1

[0043] A detection method for 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzenesulfonamide,

[0044] 1. Instruments and testing conditions

[0045] Shimadzu LC-15C high performance liquid chromatograph, the chromatographic column is Thermo Hypersil GOLD, the size is 4.6*250mm, 5μm;

[0046] Detector: DAD detector.

[0047] Injection volume: 20μl,

[0048] Flow rate: 1ml / min,

[0049] Detection wavelength: 230nm,

[0050] Column temperature: 25°C,

[0051] Mobile phase: KH2PO4 of mobile phase A 0.01mol / L: mobile phase B acetonitrile, adopt gradient elution, described gradient elution condition is: 0-5min: mobile phase A 90%, mobile phase B 10%; 5-30min : mobile phase A 30%, mobile phase B 70%; 30-35min: mobile phase A 90%, mobile phase B 10%.

[0052] Diluent: Acetonitrile

[0053] Detector: DAD detector.

[0054] 2. Experimental steps

[0055] Adopt high-performance liquid chromatography to detect, and the detection steps are as follows:

[0056] (1) Accurat...

Embodiment 2

[0062]Get three batches of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl) methyl] amino] benzenesulfonamide product produced by the same production specification instruction, respectively test sample 1-3, Detect according to the detection method of embodiment 1, adopt area normalization method to carry out purity and its impurity content calculation, test result is shown in Table 1-3 and chromatogram is respectively Figure 1-3 .

[0063] Table 1 is the detection result of test product 1

[0064]

[0065]

[0066] Table 2 is the detection result of test product 2

[0067] Impurities

Peak time (min)

Peak area ratio (%)

main peak resolution

Main peak theoretical plate number

ABT31

19.227

0.82％

/

/

ABT33

19.704

99.01％

1.78

5692

maximum complex

11.777

0.06％

/

/

total miscellaneous

/

0.99％

/

/

[0068] Table 3 is the detection result of test product 3

[0069] Impurit...

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Abstract

The invention discloses a detection method of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide. A high-performance liquid chromatograph is adopted for detection, and an area normalization method is adopted for quantitative analysis, wherein chromatographic conditions include that chromatographic column is Thermo Hypersil GOLD, sample feeding amount is 15-25ul, flow rate is 0.8-1.2ml / min, column temperature is 20-30 DEG C, detection wavelength is 228-232nm, mobile phase A is 0.01mol / L KH2PO4, mobile phase B is acetonitrile, volume ratio of the mobile phase A to the mobile phaseB is (30-90):(10-70), diluent is acetonitrile, and a detector is a DAD detector. The detection method can detect purity of 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzsulfamide and impurities simply, conveniently, accurately, quickly, efficiently and reliably, has high sensitivity and is simple and convenient in operation and capable of realizing complete separation, thereby laying a foundation for research and development and quality detection of this type of compounds.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a detection method for 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzenesulfonamide. Background technique [0002] Venetoclax, ABT-199, CAS: 1257044-40-8; is a new anti-cancer drug developed by the International Cancer Research Group, which is promising to fight cancer with fewer side effects than existing drugs available for cancer treatment, Heals faster. 3-nitro-4-[[(tetrahydro-2H-pyran-4-yl)methyl]amino]benzenesulfonamide, the CAS number is 1228779-96-1, the structural formula is as follows, which is the production of ABT- It is an important intermediate of 199. The purity and size of impurities of this product directly affect the purity and large content of impurities of ABT199, and its purity directly affects the curative effect of ABT199. [0003] At present, there are no relevant literature and reports on the purity detection method of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 蒙发明曹欢燕徐亮邓超芹俞伟文樊志麒
Owner ENANTIOTECH CORP
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