Efficient Bulky Organo-Zinc Scorpionates for the Stereoselective Production of Poly(rac-lactide)s

The direct reaction of the highly sterically demanding acetamidinate-based NNN'-scorpionate protioligand Hphbptamd [Hphbptamd = N,N'-di-p-tolylbis(3,5-di-tertbutylpyrazole-1-yl)acetamidine] with one equiv. of ZnMe2 proceeds in high yield to the mononuclear alkyl zinc complex [ZnMe(?3-phbpt...

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Detalhes bibliográficos
Autores: Navarro Sanz, Marta, Garces , Andres, Sánchez-Barba Merlo, Luis Fernando, Fernández Baeza, Juan, Lara Sánchez, Agustín
Tipo de documento: artigo
Data de publicação:2021
País:España
Recursos:Universidad de Castilla-La Mancha
Repositório:RUIdeRA. Repositorio Institucional de la UCLM
OAI Identifier:oai:ruidera.uclm.es:10578/42910
Acesso em linha:https://hdl.handle.net/10578/42910
Access Level:Acceso aberto
Palavra-chave:heterotactic poly(rac-lactide)s
homogenous catalysis
rac-lactide
zinc scorpionates
Descrição
Resumo:The direct reaction of the highly sterically demanding acetamidinate-based NNN'-scorpionate protioligand Hphbptamd [Hphbptamd = N,N'-di-p-tolylbis(3,5-di-tertbutylpyrazole-1-yl)acetamidine] with one equiv. of ZnMe2 proceeds in high yield to the mononuclear alkyl zinc complex [ZnMe(?3-phbptamd)] (1). Alternatively, the treatment of the corresponding lithium precursor [Li(phbptamd)(THF)] with ZnCl2 yielded the halide complex [ZnCl(?3-phbptamd)] (2). The X-ray crystal structure of 1 confirmed unambiguously a mononuclear entity in these complexes, with the zinc centre arranged with a pseudotetrahedral environment and the scorpionate ligand in a ?3-coordination mode. Interestingly, the inexpensive, low-toxic and easily prepared complexes 1 and 2 resulted in highly efficient catalysts for the ring-opening polymerisation of lactides, a sustainable bio-resourced process industrially demanded. Thus, complex 1 behaved as a single-component robust initiator for the living and immortal ROP of rac-lactide under very mild conditions after a few hours, reaching a TOF value up to 5520 h-1 under bulk conditions. Preliminary kinetic studies revealed apparent zero-order dependence on monomer concentration in the absence of a cocatalyst. The PLA materials produced exhibited narrow dispersity values, good agreement between the experimental Mn values and monomer/benzyl alcohol ratios, as well as enhanced levels of heteroselectivity, reaching Ps values up to 0.74.