Compound 64: Tris((4-(ethoxycarbonyl)-1H-pyrazol-5-yl)oxy)lanthanum

DOI: 10.14469/hpc/11742 Metadata

Created: 2022-11-08 06:35

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)lanthanum (64): La(OTf)3 (140 mg, 0.239 mmol, 1.00 equiv) was added with stirring to pyrazolone 5 (112 mg, 0.717 mmol, 3.00 equiv) in EtOH (3.5 mL). Aqueous NaOH (2 M; 0.36 mL, 0.717 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 20 h, after which the mixture was co-evaporated to dryness with Et2O (4 x 15 mL). The residue was suspended in Et2O, and the solid collected by filtration and dried in vacuo. La-pyrazolone complex 64 (102 mg, 0.169 mmol, 71%) was obtained as a white solid, essentially pure by its 1H NMR spectrum. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of 64. 1H-NMR (400 MHz, CD3O): δ (ppm) = 7.42 (s, 1H), 3.99 (s, 2H), 1.22 – 1.12 (m, 3H). 13C{1H}-NMR (126 MHz, CD3OD): δ (ppm) = 168.8, 167.1, 140.7, 94.2, 61.1, 14.9. IR (Diamond-ATR, neat) νmax (cm-1) = 3299, 1644, 1570, 1523, 1441, 1290, 1258, 1171, 1126, 1034, 922, 783, 752, 641. m.p.: 252 – 255 °C (EtOH). Anal. Calcd for C18H21N6O9La ∙ H2O ∙ EtOH ∙ La2O3: C, 24.16; H, 2.94; N, 8.45. Found: C, 24.19; H, 2.87; N, 8.58.

Files

FilenameSizeTypeDescription
64.cdxml 10KB chemical/x-cdxml Chemdraw connection table
64.png 70KB image/png Image representation
64.cdxml 9KB chemical/x-cdxml Chemdraw connection table v2
64.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.La/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 ZBIGDMUNSLIQIT-UHFFFAOYSA-K

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