Spermineanalogue, as well as preparation method and application thereof
An analog, spermine technology, used in the field of medicine
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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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