Poly(epsilon-caprolacton) containing functional chlorine atoms and organocatalysis preparation method and application thereof
A technology for the catalytic preparation of caprolactone, which is applied in the chemical field, can solve the problems of lack of functional groups and achieve good biocompatibility
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Embodiment 1
[0042] Synthesis of Example 1P (εCL-co-αClεCL)
[0043] Synthesis of α-chloro-ε-caprolactone monomer:
[0044] Take a 500ml reaction flask with a glass joint door, weigh 2-chloro-peroxybenzoic acid (mCPBA, 36.48g, 179.6mmol) into the reaction flask. Connect the Schkenk system for three consecutive pumping cycles. Add 250ml of dichloromethane and mix well. Use a syringe to measure 2-chlorocyclohexanone (20ml, 175.1mmol) into the reactor bottle and mix evenly, react under the protection of high-purity nitrogen for 96h, 25°C;
[0045] After the reaction was completed, the reaction solution was frozen in a −20° C. refrigerator for 4 h, and then filtered with suction to remove the white solid. The filtrate was washed three times successively with saturated sodium thiosulfate solution and sodium bicarbonate solution. Note that the pH value of the sodium bicarbonate solution is not greater than 9. Wash with saturated sodium chloride solution and deionized water, respectively. D...
Embodiment 2
[0055] PCL is grafted and modified by methyl methacrylate:
[0056] Take a 10ml polymerization reaction bottle, connect it to Schlenk, bake and ventilate three times to remove water, and add dry solid poly(ε-caprolactone-co-α-chloro-ε-caprolactone) (0.5g, Cl content 0.7mmol / g×0.5g), copper powder (5.6mg, 0.0875mmol), connect the Schlenk system to evacuate and fill with argon for three times, then add DMF (4ml) into the sealed reaction bottle, mix well and then add tris(2- Dimethylaminoethyl)amine (Me 6 -TREN, 20μL, 0.0875mmol) and methyl methacrylate (MMA, 1.5ml, 14.7mmol) were mixed evenly, reacted in a water bath at 30°C for 16h, precipitated with ether, and dried under vacuum at room temperature for 12h to obtain a white solid . Dissolve the solid in DMF, precipitate it three times with ether, dry it under vacuum at room temperature, and use deuterated acetone as the solution to make 1 HNNMR characterization.
[0057] Such as image 3 As shown, the percentage content o...
Embodiment 3
[0063] Embodiment 3: PCL is modified by grafting of hydroxyethyl methacrylate:
[0064] Take a 10ml polymerization reaction bottle, connect it to Schlenk, bake and ventilate three times to remove water, and add dry solid poly(ε-caprolactone-co-α-chloro-ε-caprolactone) (0.46g, chlorine content 0.45mmol / g×0.5g), copper powder (3.46mg, 0.0525mmol), connect the Schlenk system to evacuate and fill with argon for three times, then add DMF (1.5ml) into the sealed reaction bottle, mix well and then add three (2 -Dimethylaminoethyl)amine (Me 6 -TREN, 12μL, 0.0525mmol), 2-hydroxyethyl methacrylate (HEMA, 1.5ml, 11.05mmol) were mixed evenly, reacted in a water bath at 30°C for 48h, precipitated with ether, and dried in vacuum at room temperature for 12h , to obtain a white solid. Dissolve the solid in DMF, precipitate it three times with ether, dry it under vacuum at room temperature, and use deuterated acetone as the solution to make 1 HNNMR characterization.
[0065] Such as Figu...
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