Polyethyleneglycol-aliphatic poly (ester-carbonic ester) with allyl lateral group, preparation method thereof and application thereof
A technology of allyloxycarbonyl trimethylene carbonate and polyethylene glycol, which is applied in the field of biomedical polymer materials and can solve problems such as high cost and complicated synthesis process
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Embodiment 1
[0035] Example 1: Synthesis of 2-methyl-2-allyloxycarbonyl-1,3-propanediol
[0036] 9.00 g of 2,2-dimethylolpropionic acid and 4.30 g of potassium hydroxide were dissolved in 50 ml of N,N-dimethylformamide. Stir vigorously for 1 h at 100°C to form potassium salt of 2,2-dimethylolpropionate. Propylene bromide was then added to the above solution, and stirred vigorously for 15 h at 100°C. The solvent was evaporated, the residue was dissolved in 200ml of ether, washed three times with 50ml of distilled water, and finally recrystallized with toluene to obtain 7.9g of 2-methyl-2-allyloxycarbonyl-1,3-propanediol with a yield of 68%. Its structure was confirmed by proton NMR spectroscopy.
Embodiment 2
[0037] Embodiment 2: the synthesis of 2-methyl-2-allyloxycarbonyl trimethylene carbonate (monomer A)
[0038] Dissolve 10 g of 2-methyl-2-allyloxycarbonyl-1,3-propanediol and 28.5 g of ethyl chloroformate in 600 ml of tetrahydrofuran, and cool in an ice-water bath. Then slowly add 28g of triethylamine into the above solution, and keep the system at about 0°C during the addition. Then react at room temperature for 10h. The precipitate was filtered off, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from tetrahydrofuran and diethyl ether to obtain 9.2 g of white crystals with a yield of 80%.
Embodiment 3
[0039] Example 3: Copolymerization of monomer A with lactic acid in the presence of polyethylene glycol
[0040] Under anhydrous and oxygen-free conditions, use methoxypolyethylene glycol (PEG) with a molecular weight of 5000 as a macromolecular initiator, take monomer A and lactide monomer, and add 1 / 200 of the total mass of the monomer Ethyl zinc was used as an initiator, stirred and reacted at 60°C for 2h, the product was dissolved in chloroform, precipitated with methanol, filtered, washed, and vacuum-dried at 35°C for 24h, to obtain polyethylene glycol, monomer A and lactic acid copolymer. Typical aggregation results are shown in Table 1.
[0041] Table 1. Copolymerization of monomer A with lactic acid in the presence of polyethylene glycol
[0042] serial number
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