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Spermineanalogue, as well as preparation method and application thereof

An analog, spermine technology, used in the field of medicine

Inactive Publication Date: 2018-06-29
TIANJIN CHASE SUN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, there is no specific drug or method for the treatment of sepsis. Clinically, the development of sepsis is mainly controlled by infection control, fluid resuscitation, booster therapy, blood sugar control, and mechanical ventilation.

Method used

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  • Spermineanalogue, as well as preparation method and application thereof
  • Spermineanalogue, as well as preparation method and application thereof
  • Spermineanalogue, as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: the preparation of impurity X

[0062] Get the buffer solution of pH6.8, every 100 milliliters dissolve 10 grams of picroamine mesylate B samples. At 37-45 degrees, TLC monitors the reaction process, and the reaction can be stopped when the main raw material disappears by more than 60%. The sample was spin-dried at 60°C, then strip-dried with 50 ml of toluene, and loaded on a silica gel column. Using ethyl acetate, n-hexane (2:1v / v) column chromatography, TLC to detect the effluent at different time periods, collect the target compound, and concentrate under reduced pressure to obtain the target compound. The purity is 99.2%, and the yield is 25%. HR-MS=545.29620 (the volume ratio of the eluent is ethyl acetate, n-hexane (2:1v / v), the amount of the eluent is 10 liters (the amount of 1g picroamine mesylate B sample used), the collection target eluent of the compound fraction,)

Embodiment 2

[0063] Embodiment 2: the preparation of impurity X

[0064] Get the buffer solution of pH6.8, every 100 milliliters dissolve 10 grams of picroamine mesylate B samples. At 37-45 degrees, TLC monitors the reaction process, and the reaction can be stopped when the main raw material disappears by more than 60%. The sample was spin-dried at 60°C and then strip-dried with 100 ml of toluene, and loaded on a silica gel column. Ethyl acetate, petroleum ether (3:1v / v) column chromatography, TLC detects the effluent at different time periods, collects the target compound, and concentrates under reduced pressure to obtain the target compound. The purity was 98.5%, and the yield was 24%. HR-MS = 545.29621. (Ethyl acetate, petroleum ether (3:1v / v) in the volume ratio of the two eluents, the amount of eluent used is 8 liters (1g of picroxamine mesylate B sample usage), collect the eluted part of the target compound liquid,)

Embodiment 3

[0065] Embodiment 3: the preparation of impurity X

[0066] Get the buffer solution of pH6.8, every 100 milliliters dissolve 10 grams of picroamine mesylate B samples. At 37-45 degrees, TLC monitors the reaction process, and the reaction can be stopped when the main raw material disappears by more than 60%. The sample was spin-dried at 60°C and then dried with 100 ml of n-butanol, and loaded on a silica gel column. Using dichloromethane, methanol (50:1v / v) column chromatography, TLC to detect the effluent at different time periods, collect the target compound, and concentrate under reduced pressure to obtain the target compound. The purity was 98.5%, and the yield was 25.2%. HR-MS=545.29619 (the volume ratio of the eluent is dichloromethane, methanol (50:1v / v), the amount of the eluent is 10 liters (the amount of 1g picrochloramine mesylate B used), and the target compound is collected part of the eluate,)

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Abstract

The invention belongs to the technical field of medicines, and concretely relates to a spermineanalogue, as well as a preparation method and application thereof. The invention discloses an oxydative degradation impurity X of kukoamineBmesylate, a preparation method thereof, application of the oxydative degradation impurity X used as a content detection reference compound for kukoamine B mesylate content detection, and a detection method.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a spermine analogue and its preparation method and application. Background technique [0002] Sepsis is a systemic inflammatory response syndrome (Systemic Inflammatory Response Syndrome, SIRS) caused by infection, which can be divided into sepsis, severe sepsis, and septic shock according to the severity, and can eventually lead to multiple organ dysfunction syndrome (MODS), which is the leading cause of death in intensive care unit (ICU) patients. Despite the continuous advancement of science and technology in the medical and health field, the level of ICU critical care technology has been greatly improved, but sepsis is still an unsolved problem in the medical field, with high morbidity (about 50-95 / 100,000) and high mortality. (up to 70%), high treatment costs are always threatening human health. Currently, there is no effective drug or method for treating seps...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C235/78G01N30/02G01N30/06
CPCC07C231/12C07C235/78G01N30/02G01N30/06G01N2030/067
Inventor 张存彦张泽宇韩冬刘畅李宝齐郭新荣王贵霞刘登科孔凯郭嘉林董凯
Owner TIANJIN CHASE SUN PHARM CO LTD