Polymerized vitamin C acrylic ester high molecular material and preparation method thereof
A polymer material and acrylate technology, which is applied in the field of polyvitamin C acrylate material and its preparation, can solve the problems of low polymerization ability, etc., and achieve the effect of rapid reaction, strong polymerization reaction activity, and no molecular residue
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Embodiment 1
[0028] 1) Under the protection of nitrogen, add vitamin C (10.5g, 60mmol), potassium carbonate (20.7g, 150mmol) and N,N'-dimethylformamide (40mL) to a 100mL three-necked flask in sequence. After 2 hours of reaction, a mixed solution of benzyl bromide (23.9 g, 140 mmol) and N, N'-dimethylformamide (30 mL) was added dropwise, and the reaction was continued for 8 hours. The reaction solution was washed with deionized water, and the organic phase was collected. , dried, concentrated, and separated by column chromatography to obtain product II;
[0029]
[0030] 2) Add acryloyl chloride dropwise to a 100ml three-necked flask containing compound II (10.6g, 30mmol), triethylamine (3.6g, 36mmol) and anhydrous dichloromethane (50mL) at 0°C under nitrogen protection (3.0g, 33mmol) and dichloromethane (20mL) mixed solution, reacted for 8 hours, the reaction solution was washed with deionized water, dried, concentrated, and separated by column chromatography to obtain compound III;
...
Embodiment 2
[0041] 1) with embodiment 1 step 1)
[0042] 2) with embodiment 1 step 2)
[0043] 3) with embodiment 1 step 3)
[0044] 4) Under nitrogen protection, azobiscyanovaleric acid (14mg, 0.05mmol), compound IV (70mg, 0.25mmol), compound III (1.6g, 4mmol) and dioxane were sequentially added to a 25mL reaction flask (3mL), the reaction system was placed in an 80°C oil bath and stirred for 20 hours, and the reaction solution was concentrated and precipitated in anhydrous ether (100mL) to obtain polymer V;
[0045]
[0046] In the formula, n=90.
[0047]5) Add polymer V (600mg), palladium carbon (480mg), tetrahydrofuran (10ml) methanol (10mL) to a 50ml single-necked bottle successively, under hydrogen atmosphere, stir at room temperature for 15 hours, filter, concentrate, and dissolve in anhydrous Precipitate in diethyl ether (100mL) to obtain product I;
[0048]
[0049] In the formula, n=90.
[0050] When the polymer obtained in Examples 1 and 2 is 1.0 mM and 2.0 mM when t...
Embodiment 3
[0052] 1) with embodiment 1 step 1)
[0053] 2) with embodiment 1 step 2)
[0054] 3) with embodiment 1 step 3)
[0055] 4) Under nitrogen protection, azobiscyanovaleric acid (14mg, 0.05mmol), compound IV (28mg, 0.1mmol), compound III (1.64g, 4mmol) and dioxane were sequentially added to a 25mL reaction flask (3mL), the reaction system was placed in an 80°C oil bath and stirred for 20 hours, and the reaction solution was concentrated and precipitated in anhydrous ether (100mL) to obtain polymer V;
[0056]
[0057] In the formula, n=173.
[0058] 5) Add polymer V (500mg), palladium carbon (400mg), tetrahydrofuran (10ml) methanol (10mL) to a 50ml single-necked bottle successively, under hydrogen atmosphere, stir at room temperature for 20 hours, filter, concentrate, in anhydrous Precipitate in diethyl ether (100mL) to obtain product I;
[0059]
[0060] In the formula, n=173.
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