Compound 67: Tris((4-benzoyl-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)dysprosium

DOI: 10.14469/hpc/11743 Metadata

Created: 2022-11-08 06:37

Last modified: 2024-06-03 13:00

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Tris((4-benzoyl-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)dysprosium (67): Dy(OTf)3 (147 mg, 0.241 mmol, 1.00 equiv) was added with stirring to pyrazolone 10 (223 mg, 0.723 mmol, 3.00 equiv) in EtOH (5.5 mL) at 79 °C. Aqueous NaOH (2 M; 0.36 mL, 0.723 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 16 h. H2O was added (30 mL), the mixture was cooled to room temperature, and the resultant precipitate was collected by filtration, washed with H2O (3 x 10 mL) and dried in vacuo. Dy-pyrazolone complex 67 (121 mg, 0.112 mmol, 46%) was obtained as an off-white-yellow solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 67. IR (Diamond-ATR, neat) νmax (cm-1) = 1597, 1573, 1510, 1499, 1482, 1437, 1394, 1314, 1243, 1217, 1174, 1027, 898, 751, 703. HRMS (ESI) m/z: [M + H]+ calc. for (C54H46DyN6O9)+: 1086.2612, found: 1086.2613. m.p.: 182 – 184 °C (EtOH); >250 °C (decomp.). Anal. Calcd for C58H59N6O12Dy: C, 58.31; H, 4.98; N, 7.03. Found: C, 58.76; H, 4.90; N, 6.79.

Files

FilenameSizeTypeDescription
67.cdxml 17KB chemical/x-cdxml Chemdraw connection table
67.png 86KB image/png Image representation
67.mol 6KB chemical/x-mdl-molfile MDL Molfile

Member of collection / collaboration

DOIDescription
10.14469/hpc/10386 Syntheses and Characterization of Main Group, Transition Metal, Lanthanide and Actinide Complexes of Bidentate Acylpyrazolone Ligands

Subject Keywords

KeywordValue
inchi InChI=1S/3C18H16N2O3.Dy/c3*1-23-15-9-7-13(8-10-15)12-20-18(22)16(11-19-20)17(21)14-5-3-2-4-6-14;/h3*2-11,22H,12H2,1H3;/q;;;+3/p-3
inchikey RLILFBSLYDKTCT-UHFFFAOYSA-K

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