Preparation and application of polymalic acid and polybenzyl malate with high crystallinity
A technology of benzyl malate and malic acid, which is applied in dental preparations, molded cups, prostheses, etc., can solve the problems of low yield and long polymalic acid route, so as to improve the synthesis yield and shorten the polymerization time , good biocompatibility and biodegradability
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Embodiment 1
[0031] Add 12.4ml trifluoroacetic anhydride to 5g L-malic acid, stir at 0°C for 2h, the product is light yellow oily liquid, after the reaction, remove the solvent under reduced pressure, keep the flask at 0°C, the product is white solid. Dissolve the remaining solid in 63ml benzyl alcohol, stir at room temperature for 4h, dilute with 30ml ethyl acetate after the reaction is completed, and wash with 70ml 10% NaCO 3 The solution was extracted 3 times, the aqueous phase was combined, and 1mol·L -1 Adjust the pH to 7.0 with HCl, extract 3 times with 200ml ethyl acetate to remove unreacted benzyl alcohol, combine the aqueous layers, and use 1mol·L -1 Adjust the pH to 2.0 with HCl, extract three times with 150 ml ethyl acetate, combine the organic phases, wash three times with 150 ml saturated brine, dry over anhydrous magnesium sulfate, and concentrate to obtain benzyl malate monoester.
[0032] filled with N 2 Add 12g of benzyl monoester malate to the there-necked flask, dissol...
Embodiment 2
[0034] The preparation conditions of β-benzyloxycarbonyl-β-propiolactone monomer are the same as in Example 1, except that the reaction temperature for synthesizing the four-membered ring is 35°C. After the reaction is completed, the solvent is distilled off under reduced pressure to obtain a reddish-brown oil .
Embodiment 3
[0036] Remove the solvent of initiator tetraethylammonium benzoate in vacuum until white solid is separated out, fill with N 2 Add the purified β-benzyloxycarbonyl β-propiolactone, vacuumize, seal the tube, and fill with N 2 , repeated extraction three times, each vacuuming time is 2h, and the polymerization reaction is carried out at room temperature. As the polymerization reaction proceeds, the light yellow liquid gradually turns into a milky white solid. After 48 hours, vacuum-dry at 35°C to obtain β-polybenzyl malate (PMLABz) with high crystallinity.
[0037]Use X-ray diffraction to analyze the spatial distribution of atoms in PMLABz, the results are shown in figure 2 , PMLABz-1 and PMLABz-2 in the figure represent the synthesis from L-aspartic acid and L-malic acid respectively. It can be seen from the spectrum that PMLABz has obvious diffraction peaks, sharp spectral lines and high crystallinity. Compared with polybenzyl malate synthesized from L-aspartic acid, the p...
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