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

Inactive Publication Date: 2013-06-12
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hybrid compounds obtained by non-covalent bonds are prone to phase separatio...

Method used

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  • Pegylation polyoxometallate and preparation method thereof
  • Pegylation polyoxometallate and preparation method thereof
  • Pegylation polyoxometallate and preparation method thereof

Examples

Experimental program
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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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Abstract

The invention discloses pegylation polyoxometallate and preparation method thereof. According to the invention, polyethylene glycol and polyoxometallate are connected by utilizing a covalent bond mode, and a pegylated tungsten-containing polyoxometallate hybrid polymer is obtained. The method comprises the following synthesis steps: 1) reacting polyethylene glycol with succinic anhydride to obtain carboxyl polyethylene glycol; 2) carrying out an amidation reaction between the carboxyl polyethylene glycol and trihydroxymethyl aminomethane to obtain trihydroxymethyl polyethylene glycol; and 3) reacting the trihydroxymethyl polyethylene glycol and the tungsten-containing polyoxometallate to obtain the hybrid compound. The pegylated polyoxometallate hybrid compound is synthesized in the covalent bond mode. According to the synthetic method, a novel organic-inorganic hybrid compound can be obtained, the preparation method is easy and feasible, and the reaction process is easy to control, simple in purification and high in yield. According to the hybrid compound, the excellent performances of the inorganic polyoxometallate and organic polyethylene glycol are kept, so that the hybrid molecule has potential application values in the aspects of catalysis, materials, medicines and the like.

Description

technical field [0001] The present invention relates to the preparation of PEGylated polyoxometalate hybrid compounds, by which polyethylene glycols with different molecular weights can be connected to tungsten-containing polyoxometallates to obtain novel organic-inorganic hybrid compounds compound. Background technique [0002] Polyoxometalates, also known as polyoxometalates (POMs for short, polyacids for short), are a class of anionic monomolecular clusters with a definite structure formed by the transition metal atoms through oxygen coordination bridges. , of which vanadium, molybdenum, tungsten and other elements are the main representatives. Because polyoxometalates have good electron and proton transport and storage capacity, special redox potential and strong proton acidity, they are attractive in the fields of catalysis, optoelectronics, energy, materials, biology, and medicine. Therefore, it has gradually attracted widespread attention of scientists from various ...

Claims

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Application Information

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IPC IPC(8): C08G65/48
Inventor 王维唐静肖雨胡敏标侯占要王小刚
Owner NANKAI UNIV
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