Compound 68: Tris((4-(ethoxycarbonyl)-1H-pyrazol-5-yl)oxy)dysprosium (68)

DOI: 10.14469/hpc/11744 Metadata

Created: 2022-11-08 06:38

Last modified: 2024-06-03 13:00

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Tris((4-(ethoxycarbonyl)-1H-pyrazol-5-yl)oxy)dysprosium (68): Dy(OTf)3 (163 mg, 0.267 mmol, 1.00 equiv) was added with stirring to pyrazolone 5 (125 mg, 0.801 mmol, 3.00 equiv) in EtOH (6.0 mL) at 79 °C. Aqueous NaOH (2 M; 0.40 mL, 0.801 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 17 h. H2O (30 mL) was added, 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 68 (88.0 mg, 0.140 mmol, 52%) was obtained as a white solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 68. IR (Diamond-ATR, neat) νmax (cm-1) = 3329, 1636, 1560, 1522, 1512, 1457, 1437, 1314, 1245, 1172, 1124, 1037, 924, 900, 786, 753. m.p.: >250 °C (EtOH) (decomp.). Anal. Calcd for C18H21N6O9Dy ∙ 1.5 H2O ∙ EtOH: C, 34.27; H, 4.31; N, 11.99. Found: C, 34.36; H, 3.51; N, 11.90.

Files

FilenameSizeTypeDescription
68.cdxml 11KB chemical/x-cdxml Chemdraw connection table
68.png 40KB image/png Image representation
68.mol 3KB 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/3C6H8N2O3.Dy/c3*1-2-11-6(10)4-3-7-8-5(4)9;/h3*3H,2H2,1H3,(H2,7,8,9);/q;;;+3/p-3
inchikey GUZDNVPKKNEOLT-UHFFFAOYSA-K

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