Homologous Series of 2,5‐Diheptyloxy‐p‐Phenylene Vinylene (DHepO‐PV) Oligomers with Vinyl or 1‐Butenyl End Groups: Synthesis, Isolation, and Microstructure
Homologous Series of 2,5‐Diheptyloxy‐p‐Phenylene Vinylene (DHepO‐PV) Oligomers with Vinyl or 1‐Butenyl End Groups: Synthesis, Isolation, and Microstructure
复制标题
具有乙烯基或 1-丁烯基端基的 2,5-二庚氧基-对亚苯基亚乙烯基 (DHepO-PV) 低聚物的同系系列：合成、分离和微观结构
DOI：
10.1002/macp.200350006
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发表时间：
2003
影响因子：
2.5
通讯作者：
E. Thorn
中科院分区：
文献类型：
--
作者：
Ralf M. Peetz;A. Strachota;E. Thorn
本文报道了2,5-二庚氧基-对苯基乙烯（PV）低聚物的合成、分离和微观结构表征。给出并详细讨论了两个链长相关的同源系列的核磁共振和红外光谱。首先，以2,5-二庚氧基-1,4-二乙烯基苯为原料，采用ADMET缩聚法合成低聚物。schrock型烷基烯配合物Mo(NPhMe 2)(CHCMe 2)Ph) [OCMe(CF 3) 2] 2作为催化剂。缩聚混合物用于分离具有乙烯基端基的低聚物或作为与3-己烯的交叉复分解反应的进料组分，产生具有1-丁基端基的热稳定衍生物（研究温度高达250°C）。从低聚物混合物中，用柱层析法分离出单低聚物至八聚体（n=2…8）。单分散性采用MALDI-TOD质谱法测定。同源系列的颜色跨度很大，从无色（单体）到黄色（三聚体）到红色（六聚体及以上）。详细分析了核磁共振谱的链长依赖性。所提出的数据也可用于模拟聚合物体系的有价值的参考化合物。
In this paper we report the synthesis, isolation, and microstructure characterization of 2,5-diheptyloxy-p-phenylene vinylene (PV) oligomers. Two homologous series with their chain length dependent NMR and IR spectra are presented and discussed in detail. To obtain the products, first, oligomer mixtures were synthesized by acyclic diene metathesis (ADMET) polycondensation of 2,5-diheptyloxy-1,4- divinylbenzene. The Schrock-type alkylidene complex (Mo(NPhMe 2 )(CHCMe 2 )Ph) [OCMe(CF 3 ) 2 ] 2 served as a catalyst. The polycondensation mixture was used either for the isolation of the oligomers with vinyl end groups or as a feed component for a cross metathesis reaction with 3-hexene yielding thermally stable derivatives (investigated up to 250°C) with 1-butenyl end groups. From the oligomer mixtures, single oligomers up to the octamer (n=2...8) were isolated by means of column chromatography. The monodispersity was determined by means of MALDI-TOD mass spectrometry. The colors within the homologous series span widely from colorless (monomer to yellow (trimer) to red (hexamer and upwards). The chain-length dependence of the NMR spectra is resolved in detail. The presented data could also be used for valuable reference compounds for analogue polymer systems.