Double-chain structured polyethylene glycol derivative preparation and its combination with pharmaceutical molecule
A technology of polyethylene glycol and drug molecules, applied in the field of active derivatives of polyethylene glycol, can solve the problems of protein inactivation, hydrolysis of linking groups, loss of favorable properties, etc.
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Embodiment 1
[0034] Preparation of Dipolyethylene Glycol Thio S-ester Lipoic Acid Succinimide Ester
[0035] Reaction formula:
[0036]
[0037]Take 10g of monomethoxy polyethylene glycol acid 5000 (0.002mol) and dissolve it in 50ml of dichloromethane, add an appropriate amount of thionyl chloride, stir at room temperature for 5-7 hours, and remove the solvent and the remaining thionyl chloride by rotary evaporation , Dissolve the obtained solid in 75ml of dichloromethane, then add 0.21g lipoic acid (reduced form) (0.001mol) and 0.40g pyridine (0.005mol), stir and reflux for 16-24 hours. Filtrate and evaporate the resulting filtrate to dryness under reduced pressure, dissolve the solid in 50ml of dichloromethane, then add 0.58g of N-hydroxysuccinimide (0.005mol), in dimethylaminopyridine (DMAP) and dicyclohexylcarbodi In the presence of imine (DCCI), react at -20~10°C for 4 hours or overnight. Use a water separator to remove water, continue to reflux overnight, and then remove the dic...
Embodiment 2
[0039] Preparation of Dipolyethylene Glycol Thio S-ester Lipoic Acid Maleimide Ester
[0040] Reaction formula:
[0041]
[0042] Take 16g of monomethoxy polyethylene glycol acid 8000 (0.002mol) and dissolve it in 50ml of dichloromethane, add an appropriate amount of thionyl chloride, stir at room temperature for 5-7 hours, and remove the solvent and the remaining thionyl chloride by rotary evaporation , The resulting solid matter was dissolved in 75ml of dichloromethane, then added 0.21g of lipoic acid (reduced form) (0.001mol) and 0.40g of pyridine (0.005mol), and stirred and refluxed for 16 hours. Filtrate and evaporate the resulting filtrate to dryness under reduced pressure, dissolve the solid in 50ml of dichloromethane, then add 0.57g of N-hydroxy maleimide (0.005mol), in dimethylaminopyridine (DMAP) and dicyclohexyl carbon In the presence of diimine (DCCI), react at -20~10°C for 4 hours or overnight. Use a water separator to remove water, continue to reflux overnig...
Embodiment 3
[0044] Preparation of Dipolyethylene glycol thioether lipoic acid succinimidyl ester
[0045] Reaction formula:
[0046]
[0047] Take 20g of monomethoxypolyethylene glycol 10000 (0.002mol) and dissolve it in 50ml of dichloromethane, add an appropriate amount of thionyl chloride, stir at room temperature for 5-7 hours, remove the solvent and the remaining thionyl chloride by rotary evaporation, The obtained solid matter was dissolved in 75ml of dichloromethane, and then 20ml of ethanol solution of 0.21g lipoic acid (reduced form) (0.001mol) and 0.20g NaOH (0.005mol) was added, and the pH was adjusted with hydrochloric acid after stirring and reflux for 18-24 hours value to 5.0. The mixture solvent was evaporated to dryness under reduced pressure, and the solid was dissolved in 50ml of dichloromethane, and then 0.58g of N-hydroxysuccinimide (0.005mol) was added, and in dimethylaminopyridine (DMAP) and dicyclohexylcarbodiimide In the presence of (DCCI), react at -20~10°C fo...
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