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Monomeric Tris(η2-pyrazolato)Lanthanoid Complexes with the Bulky 3,5-Di(tert-butyl)pyrazolato Ligand

✍ Scribed by Joanna E. Cosgriff; Dr. Glen B. Deacon; Dr. Bryan M. Gatehouse; Dipl.-Chem. Holger Hemling; Prof. Dr. Herbert Schumann

Publisher: John Wiley and Sons
Year: 1993
Tongue: English
Weight: 291 KB
Volume: 32
Category: Article
ISSN: 0044-8249
DOI: 10.1002/anie.199308741

No coin nor oath required. For personal study only.

✦ Synopsis

1,3.5-Tris[diazo(3-(diazo(3-(diazo(phenyl)methyl)phenyl)methyl)phenyl)methyllbenzene (4d):

The nonaketone 4 b was converted to the corresponding nonahydrazone 4 c by the addition of anhydrous hydrazine and hydrazine hydrochloride in dimethyl sulfoxide (DMSO) at 90'C. The nonahydrazone 4c was then oxidized with HgO in a benzene/CH,CI, mixture in the presence of a 3 M solution of KOH in ethanol. The mixture was stirred for 7 days at room temperature. Filtration of the reaction mixture followed by concentration of the filtrate in vacuo left a deep wine-red oil, which was immediately chromatographed on alumina (Woelm neutral, activity IV) at 0 'C with hexane and benzene. This afforded the nonadiazo compound 4 d as a deep red oil in 65%

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