Pegylation polyoxometallate and preparation method thereof
A polyoxometalate and PEGylation technology, applied in the field of PEGylated polyoxometalate and its preparation, can solve problems such as unstable properties and phase separation, and achieve easy reaction, mild conditions, enhanced The effect of stability
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Embodiment 1
[0028] The average molecular weight of polyethylene glycol is 1000, one end is -OH, and the other end is -OCH 3 .
[0029] 1) Synthesis of carboxypolyethylene glycol
[0030] Under the protection of argon, 8 g of polyethylene glycol 1000, 1.2 g of succinic anhydride, and 0.98 g of 4-dimethylaminopyridine were dissolved in 50 mL of anhydrous toluene, stirred and heated to 80° C., and reacted for 12 h. After the reaction, it was spin-dried, dissolved in dichloromethane, and extracted successively with aqueous hydrochloric acid at pH=2 and saturated aqueous sodium chloride. The organic phase was collected, dried overnight with anhydrous sodium sulfate, then suction-filtered, concentrated, precipitated in ether, and dried in vacuo to obtain 5.0 g of a white solid with a yield of 56.8%.
[0031] 2) Synthesis of trimethylol polyethylene glycol
[0032] Under the protection of argon, dissolve 0.5g carboxypolyethylene glycol 1000, 0.15g 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinolin...
Embodiment 2
[0036] The average molecular weight of polyethylene glycol is 2000, one end is -OH, and the other end is -OCH 3 .
[0037] 1) Synthesis of carboxypolyethylene glycol
[0038] Under the protection of argon, 5 g of polyethylene glycol 2000, 0.38 g of succinic anhydride, and 0.32 g of 4-dimethylaminopyridine were dissolved in 50 mL of anhydrous toluene, stirred and heated to 80° C., and reacted for 12 h. After the reaction, it was spin-dried, dissolved in dichloromethane, and extracted successively with aqueous hydrochloric acid at pH=2 and saturated aqueous sodium chloride. The organic phase was collected, dried overnight with anhydrous sodium sulfate, then suction-filtered, concentrated, precipitated in ether, and dried in vacuo to obtain 4.5 g of a white solid with a yield of 85.7%.
[0039] 2) Synthesis of trimethylol polyethylene glycol
[0040] Under the protection of argon, dissolve 0.4g carboxypolyethylene glycol 2000, 0.07g 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline...
Embodiment 3
[0044] The average molecular weight of polyethylene glycol is 5000, one end is -OH, and the other end is -OCH 3 .
[0045] 1) Synthesis of carboxypolyethylene glycol
[0046] Under the protection of argon, 5 g of polyethylene glycol 5000, 0.12 g of succinic anhydride, and 0.13 g of 4-dimethylaminopyridine were dissolved in 50 mL of anhydrous toluene, stirred and heated to 80° C., and reacted for 12 h. After the reaction, it was spin-dried, dissolved in dichloromethane, and extracted successively with aqueous hydrochloric acid at pH=2 and saturated aqueous sodium chloride. The organic phase was collected, dried overnight with anhydrous sodium sulfate, then suction-filtered, concentrated, precipitated in ether, and dried in vacuo to obtain 4.8 g of a white solid with a yield of 94.3%.
[0047] 2) Synthesis of trimethylol polyethylene glycol
[0048] Under the protection of argon, dissolve 0.4g carboxypolyethylene glycol 5000, 0.029g 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinol...
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