Novel derivates of camptothecin 10-position coupled bile acid
A technology of derivatives and camptothecin, applied in the field of preparation of camptothecin derivatives, can solve the problems of light and heat instability, low bioavailability, large toxic and side effects, etc., and achieve reduced toxicity, good water solubility, strong The effect of inhibition
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Embodiment 1
[0047] Embodiment 1: the synthesis of cholic acid-10-O-acetyl camptothecin:
[0048] (1) Synthesis of 10-O-ethyl acetate camptothecin
[0049] Add 182mg (0.5mmol) of 10-hydroxycamptothecin, 1.5mL DMF and 138mg (1mmol) of anhydrous potassium carbonate into a 25mL round-bottomed flask, stir and dissolve, then add 50μl of ethyl bromoacetate, N 2 Heated to 60°C under protection, stirred for 0.5h, and followed the reaction by TLC. After the reaction was complete, potassium carbonate was removed by filtration, concentrated in vacuo, and the resulting solid was dissolved in chloroform and methanol, separated and purified by silica gel column chromatography to obtain compound 10-O - Camptothecin ethyl acetate. Light yellow powder, yield 75%, molecular weight: 436, structural formula as follows:
[0050]
[0051] (2) Synthesis of 10-O-acetoxycamptothecin:
[0052] Into a 25 mL round bottom flask was added 218 mg (0.5 mmol) of 10-O-ethyl acetate camptothecin. Add KOH (0.1mol / L) 5...
Embodiment 2
[0060] Embodiment 2: the synthesis of deoxycholic acid-10-O-acetyl camptothecin:
[0061] (1) Synthesis of 10-O-ethyl acetate camptothecin
[0062] Same as (1) in Example 1
[0063] (2) Synthesis of 10-O-acetoxycamptothecin:
[0064] Same as (2) in embodiment 1
[0065] (3) Synthesis of methyl deoxycholate:
[0066] Add 196mg (0.5mmol) of deoxycholic acid into a 25ml three-necked flask, add 5ml of methanol to dissolve, add 100μl of acetyl chloride, and follow the reaction by TLC. After the reaction is complete, add 15ml of distilled water to precipitate a white solid, filter, and dry in vacuo to obtain the target product. The yield is 95%; the molecular weight is 406; the structural formula is as follows:
[0067]
[0068] (4) Synthesis of deoxycholic acid-10-O-acetylcamptothecin: (A2)
[0069] In a 25ml three-necked flask, 204mg (0.5mmol) of 10-acetoxycamptothecin, 406mg (1mmol) of methyl deoxycholate, 1-[(3-dimethylamino)propyl]-3-ethylcarbonyl Amine hydrochloride (...
Embodiment 3
[0071] Embodiment 3: Synthesis of chenodeoxycholic acid-10-O-acetylcamptothecin:
[0072] (1) Synthesis of 10-O-ethyl acetate camptothecin
[0073] Same as (1) in Example 1
[0074] (2) Synthesis of 10-O-acetoxycamptothecin:
[0075] Same as (2) in embodiment 1
[0076] (3) Synthesis of methyl chenodeoxycholic acid:
[0077] Add 196 mg (0.5 mmol) of chenodeoxycholic acid in a 25 ml three-necked flask, add 5 ml of methanol to dissolve, add 100 μl of acetyl chloride, and follow the reaction by TLC. After the reaction is complete, add 15 ml of distilled water to precipitate a white solid, filter, and dry in vacuo to obtain the target product. Yield 96%; Molecular weight 406; Structural formula is as follows:
[0078]
[0079] (4) Synthesis of chenodeoxycholic acid-10-O-acetylcamptothecin (A3):
[0080] Add 204mg (0.5mmol) of 10-acetoxycamptothecin, 406mg (1mmol) of methyl chenodeoxycholate, and 1-[(3-dimethylamino)propyl]-3-ethylcarbonyl in a 25ml three-necked flask. Imi...
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