Temperature sensitive polymer material with biodegradability and biocompatibility and preparation method thereof
A technology of biocompatibility and polymer materials, which is applied in the field of biodegradable and biocompatible temperature-sensitive polymers and their preparation, can solve the problem of not taking into account the biodegradability and biocompatibility of polymer materials Sexual temperature-sensitive properties, inability to obtain biodegradability, biocompatibility, lack of biocompatibility and other problems, to achieve good biodegradability and biocompatibility, excellent temperature-sensitive properties, to avoid the effect of reducing or disappearing temperature-sensitive properties
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Embodiment 1
[0044] Embodiment 1: the preparation of poly(lysine methyl ester-diacetoxy tartaric acid)
[0045] (1) Preparation of 2,3‐diacetoxytartaric acid chloride
[0046] Add 20 g of tartaric acid and 44 ml of acetic anhydride into a round bottom flask, heat in an oil bath to 140° C., reflux for 2 h, and confirm the completion of the reaction by TLC to obtain a light yellow liquid. The light yellow liquid was cooled to crystallize the target compound. Subsequently, the crystals were washed several times with diethyl ether and dried under vacuum at 80°C to obtain 26.5 g of a white crystalline solid with a yield of 85%. Recrystallize 10 g of the crude product obtained in the previous step with a mixed solvent of acetone and petroleum ether to obtain 6.8 g of pure 2,3‐diacetoxytartaric acid, with a yield of 68%. The reaction equation is as follows:
[0047]
[0048] Add 2g of 2,3-diacetoxytartaric acid and 10ml of thionyl chloride into a 100ml single-necked bottle, and add two drop...
Embodiment 2
[0062] Embodiment 2: the preparation of poly(ethyl lysine-diacetoxy tartaric acid)
[0063] (1) Preparation of 2,3‐diacetoxytartaric acid chloride
[0064] The preparation of 2,3-diacetoxy tartaric acid chloride is the same as in Example 1.
[0065] (2) Synthesis of lysine ethyl ester hydrochloride
[0066] Add 150ml of ethanol to the four-neck bottle, add 21.60ml of thionyl chloride dropwise under the condition of stirring at -10°C, and continue to react for 1h after dropping for about 1.5h. Naturally rise to room temperature to obtain 150 ml of 2 mol / l HCl ethanol solution. Transfer the above solution to a brown reagent bottle, seal it and keep it away from light for later use.
[0067] Add 50ml of ethanol to the four-neck bottle, and slowly add 12ml of thionyl chloride dropwise under the condition of stirring at -10°C. The dropping time is about 20min, and the stirring is continued for 1h after the dropping is completed. Add 5 g of lysine hydrochloride and heat to reflu...
Embodiment 3
[0077] Embodiment 3: the preparation of poly(lysine methyl ester-diethoxytartaric acid)
[0078] (1) Preparation of 2,3‐diethoxytartaric acid chloride
[0079] 4.6g of sodium tartrate and 10ml of ethyl bromide under the action of 0.2g of sodium hydride (or sodium amide) as a catalyst to obtain 2,3-diethoxydiethyl tartrate, the resulting product is acidified and hydrolyzed with dilute hydrochloric acid for 3 hours to obtain 2,3‐diethoxytartaric acid. 2,3-diethoxy tartaric acid was refluxed with thionyl chloride under the catalysis of DMF for 1.5h. After separation and purification, 2,3-diethoxy tartaric acid chloride monomer was obtained with a yield of 45 %.
[0080]
[0081] (2) Synthesis of lysine methyl ester hydrochloride
[0082] The synthetic method of lysine methyl ester hydrochloride is with embodiment 1.
[0083] (3) Preparation of thermosensitive poly(lysine methyl ester‐diethoxy tartaric acid)
[0084] Add 10ml of methanol into the reaction bottle, and cool ...
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