Polyethylene glycol-cyclooctyne derivatives
A polyethylene glycol and derivative technology, applied in the field of gel, polyethylene glycol-cyclooctyne active derivatives, can solve the problems of non-water solubility and limited application
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Embodiment 1
[0072] Example 1: Preparation of Polyethylene Glycol (5000Da)-(Cyclooctyne-2-Oxygen)-Acetamide
[0073]
[0074] Dissolve 0.87g of cyclooctyne-2-oxoacetic acid and 0.64g of N-hydroxysuccinimide (NHS) in 20ml of dichloromethane, and add N,N'-dicyclohexylcarbodiimide ( DCC) 1.22g, reacted for 4h, dissolved 10.0g of polyethylene glycol (5000Da)-ethylamine in 80ml of dichloromethane, added to the reaction bottle, reacted overnight, filtered, concentrated at 40°C, heated to dissolve the ice with 150ml of isopropanol Precipitate in a water bath, filter, wash the filter cake twice with isopropanol, and dry in vacuum to obtain 9.3 g of polyethylene glycol (5000 Da)-(cyclooctyne-2-oxy)-acetamide.
[0075] 1 H-NMR (DMSO) δ: 1.44-2.33 (m, CH 2 ring,20H),4.26(m,CH ring,2H)
Embodiment 2
[0076] Example 2: Preparation of methoxypolyethylene glycol (5000Da)-(cyclooctyne-2-oxo)-acetamide
[0077]
[0078] Dissolve 0.44g of cyclooctyne-2-oxoacetic acid and 0.34g of N-hydroxysuccinimide (NHS) in 10ml of dichloromethane, and add N,N'-dicyclohexylcarbodiimide ( DCC) 0.62g, react for 4h, dissolve 10.0g of methoxypolyethylene glycol (5000Da)-ethylamine in 90ml of dichloromethane, add to the reaction bottle, react overnight, filter, concentrate at 40°C, and use 150ml of isopropanol Heat to dissolve the precipitate in an ice-water bath, filter, wash the filter cake twice with isopropanol, and vacuum-dry to obtain 9.5 g of methoxypolyethylene glycol (5000 Da)-(cyclooctyne-2-oxo)-acetamide.
[0079] 1 H-NMR (DMSO) δ: 1.44-2.33 (m, CH 2 ring,10H),4.26(m,CH ring,1H)
Embodiment 3
[0080] Example 3: Preparation of methoxypolyethylene glycol (10000Da)-ethylcarbamate-(bicyclo[6.1.0]nonon 4-yne)-9-methyl ester
[0081]
[0082] Dissolve 1.0 g of methoxypolyethylene glycol (10000 Da)-ethylamine in 10 ml of dichloromethane, and under nitrogen protection, (bicyclo[6.1.0]nonon 4-yne)-9-methoxycarbonyl-succinyl imidate Add 0.032g into the reaction flask, react overnight, filter, concentrate at 40°C, heat with 20ml of isopropanol to dissolve the precipitate in an ice-water bath, filter, wash the filter cake twice with isopropanol, and dry in vacuum to obtain methoxypolyethylene glycol (10000Da 0.9 g of )-ethylcarbamate-(bicyclo[6.1.0]nonon-4-yne)-9-methyl ester.
[0083] 1 H-NMR(DMSO)δ: 0.86-2.23(m, CH 2 ring,8H),1.26(t,CH,1H),4.01(d,CH 2 -O,2H)
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