Camptothecin 20- position cholic acid derivative and preparation method thereof
A derivative, camptothecin technology, applied in the field of preparation of camptothecin derivatives, can solve problems such as poor targeting, light and heat instability, poor solubility, etc., to increase bioavailability, maintain pharmacological activity, reduce toxic effect
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Embodiment 1
[0042] Embodiment 1: cholic acid-20-O-glutamic acid-camptothecin synthesis:
[0043] (1) Synthesis of 20-O-camptothecin glutamate:
[0044] Add 174mg (0.5mmol) of camptothecin, 303mg (1mmol) of N-tert-butoxycarbonyl-glutamic acid 5-tert-butyl ester, 1-[(3-dimethylamino)propyl]-3 in a 25ml three-necked flask -Ethylcarbimide hydrochloride (EDCI) 286.5mg (1.5mmol), 4-dimethylaminopyridine (DMAP) 18mg (0.17mmol), anhydrous dichloromethane 10ml, stirring at room temperature for 3.5 hours, by TLC Track reactions. After the reaction was complete, 20ml of chloroform was added to the reaction solution, followed by 50ml of water, 50ml of saturated NaHCO 3 The solution was washed 3 times with anhydrous MgSO 4 Dry, filter under reduced pressure to remove MgSO 4 Concentrate under reduced pressure, add hydrochloric acid methanol solution to dissolve, stir at room temperature for 3 hours, follow the reaction by TLC, and concentrate under reduced pressure after the reaction is complete. ...
Embodiment 2
[0052] Embodiment 2: Synthesis of deoxycholic acid-20-O-glutamic acid-camptothecin:
[0053] (1) Synthesis of 20-O-camptothecin glutamate:
[0054] The method is the same as example 1(1)
[0055] (2) Synthesis of deoxycholic acid activated ester:
[0056] In a 25ml three-necked flask, add deoxycholic acid 196 (0.5mmol), N-hydroxysuccinimide 172.5mg (1.5mmol), 1-[(3-dimethylamino)propyl]-3-ethylcarbonyl Imine hydrochloride (EDCI) 286.5 mg (1.5 mmol), anhydrous dichloromethane 10 ml, stirred at room temperature for 3 hours, followed by TLC reaction. After the reaction was complete, 20ml of chloroform was added to the reaction solution, followed by 50ml of water, 50ml of saturated NaHCO 3 The solution was washed 3 times with anhydrous MgSO 4 Dry, filter under reduced pressure to remove MgSO 4 After concentrating under reduced pressure, 153 mg of white solid was obtained, with a yield of 64.9%; molecular weight 489; structural formula is as follows:
[0057]
[0058] (3) ...
Embodiment 3
[0061] Embodiment 3: Synthesis of ursodeoxycholic acid-20-O-glutamic acid-camptothecin:
[0062] (1) Synthesis of 20-O-camptothecin glutamate:
[0063] The method is the same as example 1(1)
[0064] (2) Synthesis of ursodeoxycholic acid activated ester:
[0065] In a 25ml three-necked flask, add deoxycholic acid 196 (0.5mmol), N-hydroxysuccinimide 172.5mg (1.5mmol), 1-[(3-dimethylamino)propyl]-3-ethylcarbonyl Imine hydrochloride (EDCI) 286.5 mg (1.5 mmol), anhydrous dichloromethane 10 ml, stirred at room temperature for 3 hours, followed by TLC reaction. After the reaction was complete, 20ml of chloroform was added to the reaction solution, followed by 50ml of water, 50ml of saturated NaHCO 3 The solution was washed 3 times with anhydrous MgSO 4 Dry, filter under reduced pressure to remove MgSO 4 Concentrate under reduced pressure to obtain a white solid with a yield of 77%; the molecular weight is 489; the structural formula is as follows:
[0066]
[0067] (3) Synt...
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