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Lithium, sodium, potassium and calcium amine-bis(phenolate) complexes in the ring-opening polymerization of rac-lactide.
Dalton Transactions ( IF 3.5 ) Pub Date : 2020-01-13 , DOI: 10.1039/c9dt04561a Katalin Devaine-Pressing 1 , Fabio J Oldenburg 1 , Jan P Menzel 1 , Maximilian Springer 1 , Louise N Dawe 2 , Christopher M Kozak 1
Dalton Transactions ( IF 3.5 ) Pub Date : 2020-01-13 , DOI: 10.1039/c9dt04561a Katalin Devaine-Pressing 1 , Fabio J Oldenburg 1 , Jan P Menzel 1 , Maximilian Springer 1 , Louise N Dawe 2 , Christopher M Kozak 1
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Compounds of Li, Na, K and Ca of a tetradentate amino-bis(phenolato) ligand were prepared. Bimetallic compounds formulated as M2[L](THF)n (where M = Na, n = 1 (1·THF) or Li, n = 1 (2·THF)) were synthesized via the reaction of H2[L] (where [L] = 2-pyridylmethylamino-N,N-bis(2-methylene-4-methoxy-6-tert-butylphenolato) with sodium hydride or n-butyllithium, respectively, in THF. Monometallic complexes MH[L](THF)n (where M = Na, n = 1 (3·THF), Li, n = 0 (4) and K, n = 0 (5)) were obtained by reaction of H2[L] with MN(SiMe3)2 where M = Na, Li, or K. Calcium complex Ca[L](THF) (6·THF) was synthesized in two ways; reaction of Na2[L] with calcium iodide in THF, and reaction of Ca[N(SiMe3)2]2 with H2[L] in toluene. Compounds 1-6 exhibit activity for rac-lactide polymerization under melt and solution conditions. Moderate control of polymer molecular weights was achieved in toluene, whereas polydisperse polymer was obtained under solvent free conditions. MALDI-TOF MS analysis of the polymer end groups revealed a predominantly cyclic nature for the polylactides.
中文翻译：
锂，钠，钾和钙胺-双（酚盐）配合物在外消旋丙交酯的开环聚合中。
制备了四齿氨基双（酚基）配体的Li，Na，K和Ca的化合物。通过H2 [L]（其中M = Na，n = 1（1·THF）或Li，n = 1（2·THF））合成为M2 [L]（THF）n的双金属化合物。 [L] = 2-吡啶基甲基氨基-N，N-双（2-亚甲基-4-甲氧基-6-叔丁基苯酚基）与氢化钠或正丁基锂在THF中的混合物。单金属配合物MH [L]（THF）通过H2 [L]与MN（SiMe3）2反应得到n（其中M = Na，n = 1（3·THF），Li，n = 0（4）和K，n = 0（5）） M = Na，Li或K。钙络合物Ca [L]（THF）（6·THF）的合成方法有两种：Na2 [L]与碘化钙在THF中的反应以及Ca [N（SiMe3）在甲苯中具有H2 [L]的2] 2化合物1-6在熔融和溶液条件下均具有外消旋丙交酯聚合的活性。在甲苯中实现了对聚合物分子量的适度控制，而在无溶剂条件下获得了多分散聚合物。聚合物端基的MALDI-TOF MS分析显示，聚丙交酯具有主要的环状特性。
更新日期：2020-02-10
中文翻译：
锂，钠，钾和钙胺-双（酚盐）配合物在外消旋丙交酯的开环聚合中。
制备了四齿氨基双（酚基）配体的Li，Na，K和Ca的化合物。通过H2 [L]（其中M = Na，n = 1（1·THF）或Li，n = 1（2·THF））合成为M2 [L]（THF）n的双金属化合物。 [L] = 2-吡啶基甲基氨基-N，N-双（2-亚甲基-4-甲氧基-6-叔丁基苯酚基）与氢化钠或正丁基锂在THF中的混合物。单金属配合物MH [L]（THF）通过H2 [L]与MN（SiMe3）2反应得到n（其中M = Na，n = 1（3·THF），Li，n = 0（4）和K，n = 0（5）） M = Na，Li或K。钙络合物Ca [L]（THF）（6·THF）的合成方法有两种：Na2 [L]与碘化钙在THF中的反应以及Ca [N（SiMe3）在甲苯中具有H2 [L]的2] 2化合物1-6在熔融和溶液条件下均具有外消旋丙交酯聚合的活性。在甲苯中实现了对聚合物分子量的适度控制，而在无溶剂条件下获得了多分散聚合物。聚合物端基的MALDI-TOF MS分析显示，聚丙交酯具有主要的环状特性。
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