Camptothecin derivative and its preparation
A technology of derivatives and camptothecin, which is applied in the field of preparation of camptothecin derivatives, can solve the problems of light and heat instability, poor solubility, large toxic and side effects, etc., to achieve reduced toxicity, good water solubility, and maintain pharmacological activity Effect
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Embodiment 1
[0073] 10-O-(3-pyridinium salt) propyl camptothecin
[0074] (1) Synthesis of 10-O-(3-bromo)propyl camptothecin
[0075] Add 182.18mg (0.5mmol) of 10-hydroxycamptothecin in a 25mL round bottom flask, 1.5mL DMSO and 345.94mg (2.5mmol) of anhydrous potassium carbonate, after stirring and dissolving, add 0.86mL of 1,3-dibromopropane ( 10.01mmol), N 2 Heated to 60°C under protection, stirred for 72 hours, and followed the reaction by TLC. After the reaction was complete, the reaction liquid was poured into water, and the solid was precipitated, filtered, and the obtained solid was dissolved in chloroform and methanol with a volume fraction of 8:2, and passed through a silica gel column. Separation and purification by chromatography, and gradient elution with chloroform-methanol (100:1-100:3) gave compound 10-O-(3-bromo)propylcamptothecin. The molecular weight of the compound is: 484.06, and the structural formula is as follows:
[0076]
[0077] (2) Synthesis of 10-O-(3-pyri...
Embodiment 2
[0081] 10-O-(3-(3-acetyl)pyridinium salt-1)propylcamptothecin
[0082] (1) The synthetic method of 10-O-(3-bromo) propyl camptothecin is identical with embodiment 1 (1)
[0083] (2) Synthesis of 10-O-(3-(3-acetyl)pyridinium salt-1)propylcamptothecin
[0084] Add compound 10-O-(3-bromo)propyl camptothecin 97.07mg (0.2mmol) and excess 3-acetylpyridine in a 25mL round bottom flask, heat to 50°C, stir for 12h, track the reaction by TLC, the product The Rf value developed in methanol is zero. After the reaction is complete, trichloromethane is added to the reaction solution to precipitate a yellow solid product, which is filtered, washed fully with trichloromethane, and vacuum-dried at 60°C to obtain the product 10-O-(3-( 3-acetyl)pyridinium salt-1) propylcamptothecin. The compound is light yellow powder, 95.10mg, molecular weight: 526.20; m.p.192°C, yield 90.4%. The structural formula is as follows:
[0085]
Embodiment 3
[0087] 10-O-(3-(3-hydroxy)pyridinium salt-1)propylcamptothecin
[0088] (1) The synthetic method of 10-O-(3-bromo) propyl camptothecin is identical with embodiment 1 (1)
[0089] (2) Synthesis of 10-O-(3-(3-hydroxy)pyridinium salt-1)propylcamptothecin
[0090] Add compound 10-O-(3-bromo)propyl camptothecin 97.07mg (0.2mmol), 1.5mL DMSO and excess 3-phenolhydroxypyridine into a 25mL round bottom flask, heat to 50°C to dissolve the reactant, and stir for 12h , the reaction was tracked by TLC, the Rf value of the product developed in methanol was zero, after the reaction was complete, an appropriate amount of chloroform was added to the reaction solution, and a yellow solid product was precipitated, filtered, and fully washed with a mixture of chloroform and methanol in an appropriate proportion , 60 ℃ vacuum drying to obtain the product 10-O-(3-(3-hydroxy) pyridinium salt-1) propyl camptothecin. The compound is light yellow powder, 80.4mg, m.p.293°C, molecular weight: 500.18; ...
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