Direct access to biocompatible nitroxide containing polymers†,Polymer Chemistry

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Direct access to biocompatible nitroxide containing polymers†
Polymer Chemistry ( IF 4.1 ) Pub Date : 2018-02-26 00:00:00 , DOI: 10.1039/c8py00089a
Christiane Lang _{1,

2,

3,

4,

5} , Leonie Barner _{1,

2,

3,

4,

5} , James P. Blinco _{1,

2,

3,

4,

5} , Christopher Barner-Kowollik _{1,

2,

3,

4,

5} , Kathryn E. Fairfull-Smith _{1,

2,

3,

4,

5}

Affiliation

We introduce the preparation and ring-opening polymerization of a nitroxide containing carbonate monomer. Using 1,8-diazabicyclo undec-7-ene (DBU) and a thiourea as the catalyst system, we demonstrate that the free radical moiety of the monomer has no influence on the ring-opening copolymerization with D/L-lactide in a wide range of compositions between 10% and 80% of the nitroxide monomer, which can be readily controlled by the comonomer composition in the polymerization mixture. The copolymers exhibit narrow and monomodal mass distributions with number average molar masses between 6000 g·mol⁻¹ to 7000 g·mol⁻¹ and low dispersities below 1.1. The free radical functionality is retained during the polymerization as demonstrated by electron spin resonance (EPR) spectroscopy. High-resolution mass spectrometry coupled to size exclusion chromatography allowed an in-depth analysis of the copolymers showing well-defined linear polymer chains with excellent endgroup fidelity. Furthermore, the molar mass of the polymers was controlled by the monomer to initiator ratio which led to copolymers of up to 19 500 g·mol⁻¹.

中文翻译：

直接获得含生物相容性一氧化氮的聚合物†

我们介绍了含氮氧化物的碳酸酯单体的制备和开环聚合。使用1,8-二氮杂双环十一碳烯（DBU）和硫脲作为催化剂体系，我们证明了单体的自由基部分对D / L-丙交酯在宽范围内的开环共聚没有影响。范围为氮氧化物单体的10％至80％之间的范围，可以容易地通过聚合混合物中的共聚单体组成来控制。共聚物表现出窄的和单峰的质量分布，数均摩尔质量为6000 g·mol ^-1至7000 g·mol ^-1低于1.1的低分散度。如电子自旋共振（EPR）光谱所示，自由基官能团在聚合过程中得以保留。高分辨率质谱分析法与尺寸排阻色谱法相结合，可以对共聚物进行深入分析，显示出定义明确的线性聚合物链，并具有出色的端基保真度。此外，聚合物的摩尔质量由单体与引发剂的比率控制，这导致共聚物高达19 500 g·mol ^-1。

更新日期：2018-02-26

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