Organometallic Complexes of Palladium(II) Derived from 2,6-Diacetylpyridine Dimethylketal
摘要：
PdCl2 reacts with 2,6-diacetylpyridine (dap) (1:1) in refluxing MeOH to give the pincer complex [Pd(O1,N1,C1-L)Cl] (1) and (QH)2[{PdCl2(μ-Cl)}]2 (2), where L is the monoanionic ligand resulting from deprotonation of the acetyl methyl group of the monoketal of dap and QH is C5H3NH{C(OMe)2Me}2-2,6, the diketal of Hdap+. Reaction of 2 with NEt3 (1:2) in MeOH affords Q = C5H3N{C(OMe)2Me}2-2,6 (3). Complex 1 reacts with 2 equiv of RNC at 0 °C to give trans-[Pd(C1-L)Cl(CNR)2] (R = Xy = 2,6-dimethylphenyl (4a), tBu (4b)) but at room temperature affords [Pd(O2,C2-LR)Cl(CNR)] (R = Xy (5a), tBu (5b)). The ligand LR results from the insertion of one isocyanide into the PdC bond plus a tautomerization process from β-ketoimine to β-ketoenamine and coordinates in 5 through the carbonyl oxygen atom (O2) and the inserted isocyanide carbon atom (C2). The reaction of 1 with 1 equiv of RNC at 0 °C leads to a mixture of [Pd(N1,C1-L)Cl(CNR)] (R = Xy (6a), tBu (6b); 8590%), 1, and 4, but at room temperature gives the pincer ...
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关键词：
conjugate vaccines glycoconjugates Haemophilus influenzae lacto-N-neotetraose oligosaccharide synthesis thioglycosides
DOI：
10.1021/om100079x
被引量：
年份：
2010
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