Multi-arm polyethylene glycol derivatives, conjugates and gels of pharmaceuticals and the same
a polyethylene glycol and derivative technology, applied in the field of multi-arm polyethylene glycol derivatives, can solve the problems of reducing the stability of the derivative, limited straight-chain polyethylene glycol derivatives with metachronous double functional groups, etc., and achieves the effect of simple structure and increased active group types
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example 1
Synthesis of 4-Arm Poly (Ethylene Glycol) Hydroxy—Single-Acetic Acid (III-1) and 4-Arm Poly(Ethylene Glycol) Hydroxy—Double-Acetic Acid (IIIA-1)
[0082]
[0083]Procedure:
[0084]4-ARM-PEG (10 kDa, 100 g) in 800 ml of TI-W was azeotropically dried by distilling off THF (20%) under nitrogen and the solution was cooled to room temperature. To the solution was added potassium tert-butoxide (4.48 g) and stirred 2 hours at room temperature. Tert-butyl bromoacetate (5.17 ml) was added dropwise and the mixture was stirred at room temperature overnight. The mixture was filtered and evaporated under vacuum to remove solvents. The residue was dissolved in a aqueous solution (H2O 500 mL+sodium hydroxide 8.16 g+sodium phosphate) and stirred 2 hours at 80° C. The PH of the aqueous solution was adjusted to about 2-3. Sodium chloride (15%) was added and the product was extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, filtered, concentrated under vacuum at 50° C., and t...
example 2
Synthesis of Four-Arm Polyethylene Glycol Hydroxy—Single-N-hydroxysuccinimidyl Ester (IV-1)
[0086]
[0087]Procedure:
[0088]4-arm poly (ethylene glycol) hydroxy—single-acetic acid (III-1) (10 kDa, 0.5 g) and N-hydroxysiccinimide (0.01439 g) were dissolved in dichloromethane. DCC (0.01290 g) was added and the solution was stirred overnight at room temperature, filtered, concentrated under vacuum at 40° C. The residue was dissolved in hot iso-propanol and then crystallized by cooling the solution to 0° C. The resulting precipitate was collected, washed with iso-propanol and dried to afford the 4-arm poly(ethylene glycol) hydroxy—single-N-hydroxysuccinimidyl ester (IV-1).
[0089]NMR (DMSO) δ: 2.89 (s,
[0090]
4.55 (t, CH2CH2OH).
example 3
4-Arm Poly(Ethylene Glycol) Hydroxy—Single-Methyl Acetate (IVA-1)
[0091]
[0092]Procedure:
[0093]4-arm poly (ethylene glycol) hydroxyl—single-acetic acid (III-1) (10 kDa, 3.2 g) was dissolved in methanol (16 ml). The solution was cooled to 0° C. and the concentrated sulfuric acid was added drop wise. The solution was stirred 3 hours at room temperature. The solution was adjusted PH to about 7.0 with 8% NaHCO3 anqueous solution. The product was extracted with dichloromethane. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered, and concentrated in 40° C., and then precipitated into diethyl ether. The filtrate was dried over vacuum to afford the four-arm poly(ethylene glycol) hydroxy—single methyl acetate (IVA-1).
[0094]NMR (DMSO) δ: 3.32 (s, CH2COOCH3), 4.13 (s, CH2COOCH3), 4.57 (t, CH2OH).
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