Compound 57: Syntheses and Characterization of Main Group, Transition Metal, Lanthanide and Actinide Complexes of Bidentate Acylpyrazolone Ligands

DOI: 10.14469/hpc/11738 Metadata

Created: 2022-11-08 06:24

Last modified: 2022-11-08 06:32

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Bis(ethanol) bis((4-(ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)nickel (57): NiCl2•6H2O (66.0 mg, 0.264 mmol, 1.00 equiv) was added with stirring to pyrazolone 5 (146 mg, 0.528 mmol, 2.00 equiv) in EtOH (3.5 mL) at 79 °C. After 24 h at reflux, the mixture was cooled to room temperature, and the resultant precipitate was collected by filtration and dried in vacuo. Ni-pyrazolone complex 57 (137 mg, 0.195 mmol, 74%) was obtained as a green-turquoise solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an ethanolic pyridine solution of complex 57. IR (Diamond-ATR, neat) νmax (cm-1) = 1636, 1566, 1528, 1511, 1444, 1336, 1221, 1191, 1031, 803, 778. m.p.: >300 °C (EtOH) (decomp.). Anal. Calcd for C28H¬NiN4O8: C, 55.20; H, 4.96; N, 9.20. Found: C, 55.12; H, 4.78; N, 8.71.

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