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The Facile Synthesis of Lithium 2‐R‐Hydroquinolinide Complexes and Their High Activity toward ROP of ε‐Caprolactone
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2020-01-21 , DOI: 10.1002/ejic.201901309 Ziyao Fan 1 , Peng Wang 1 , Chen Wu 1 , Zhimin Liu 1 , Xia Chen 1
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2020-01-21 , DOI: 10.1002/ejic.201901309 Ziyao Fan 1 , Peng Wang 1 , Chen Wu 1 , Zhimin Liu 1 , Xia Chen 1
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Four lithium 2‐R‐hydroquinolinide complexes [1‐(2‐(R)‐C9H7)NLi·THF2]2 (1 R = Me, 2 R = nBu) and [1‐(8‐(Me)‐2‐(Bun)‐C9H6)NLi·X]2 (3 X = THF, 4 X = Et2O) were prepared by the nucleophilic addition reaction of quinoline and 8‐methylquinoline with MeLi or BunLi, respectively. All complexes have been characterized through NMR spectroscopy. Complexes 2–4 were determined by X‐ray crystallography. Interestingly, Li atom in 1 and 2 is tetracoordinate, whereas Li atom in 3 and 4 is three‐coordinate. All these complexes showed super‐high activity for the ring‐opening polymerization (ROP) of ε‐caprolactone in both the absence and presence of BnOH at 35 °C in CH2Cl2. By the 1–4 catalytic systems with or without BnOH as a co‐initiator, the ROP of ε‐CL proceeded well in a living manner as evidenced by the predictable molecular weights, narrow molecular weight distributions, and kinetic studies. MALDI‐TOF MS analysis revealed that the resultant PCL showed a cyclic structure in the absence of BnOH and a BnO– capped linear structure was observed in the presence of BnOH.
中文翻译：
2-R-羟基喹啉锂配合物的简便合成及其对ε-己内酯的ROP活性高
四个2-R-氢喹啉锂复合物[1-（2-（R）-C 9 H 7）NLi · THF 2 ] 2（1 R = Me，2 R = n Bu）和[1-（8-（Me ）-2-（Bu n）-C 9 H 6）NLi · X] 2（3 X = THF，4 X = Et 2 O）是通过喹啉和8-甲基喹啉与MeLi或Bu n的亲核加成反应制备的李分别。所有配合物均已通过NMR光谱表征。配合物2-4由X射线晶体学确定。有趣的是，1和2中的Li原子是四配位的，而3和4中的Li原子是三配位的。在35°C的CH 2 Cl 2中，无论是否存在BnOH，所有这些络合物均对ε-己内酯的开环聚合（ROP）具有超高的活性。通过有或没有BnOH作为共引发剂的1-4个催化体系，ε的ROP‐CL可预测的分子量，狭窄的分子量分布和动力学研究证明，CL的活生生进行得很好。MALDI-TOF MS分析显示，所得的PCL表明在不存在BnOH和BNO的环状结构-封端的线性在BnOH的存在下观察到的结构。
更新日期：2020-01-22
中文翻译：
2-R-羟基喹啉锂配合物的简便合成及其对ε-己内酯的ROP活性高
四个2-R-氢喹啉锂复合物[1-（2-（R）-C 9 H 7）NLi · THF 2 ] 2（1 R = Me，2 R = n Bu）和[1-（8-（Me ）-2-（Bu n）-C 9 H 6）NLi · X] 2（3 X = THF，4 X = Et 2 O）是通过喹啉和8-甲基喹啉与MeLi或Bu n的亲核加成反应制备的李分别。所有配合物均已通过NMR光谱表征。配合物2-4由X射线晶体学确定。有趣的是，1和2中的Li原子是四配位的，而3和4中的Li原子是三配位的。在35°C的CH 2 Cl 2中，无论是否存在BnOH，所有这些络合物均对ε-己内酯的开环聚合（ROP）具有超高的活性。通过有或没有BnOH作为共引发剂的1-4个催化体系，ε的ROP‐CL可预测的分子量，狭窄的分子量分布和动力学研究证明，CL的活生生进行得很好。MALDI-TOF MS分析显示，所得的PCL表明在不存在BnOH和BNO的环状结构-封端的线性在BnOH的存在下观察到的结构。
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