Compound 62: tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)lanthanum

Created: 2022-10-12 10:20

Last modified: 2024-11-22 09:43

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Crystal structure, NMR and IR data for Bis(aqua) tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)lanthanum (62): La(OTf)3 (129 mg, 0.220 mmol, 1.00 equiv) was added with stirring to pyrazolone 6 (153 mg, 0.659 mmol, 3.00 equiv) in EtOH (3.5 mL) at 79 °C. Aqueous NaOH (2 M; 0.33 mL, 0.659 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 20 h, after which the mixture was cooled to room temperature, the precipitate was collected by filtration and dried in vacuo. La-pyrazolone complex 62 (75 mg, 0.0901 mmol, 41%) was obtained as a yellow-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 complex 62. 1H-NMR (400 MHz, CD3OD): δ (ppm) = 7.96 (s, 1H), 7.70 – 7.63 (m, 2H), 7.40 (t, J = 7.8 Hz, 2H), 7.31 (t, J = 7.4 Hz, 1H), 4.29 (q, J = 7.1 Hz, 2H), 1.31 (t, J = 7.1 Hz, 3H). 13C{1H}-NMR (126 MHz, CD3OD): δ (ppm) = 168.5, 163.2, 140.0, 138.2, 130.0, 128.0, 123.3, 123.0, 120.5, 96.7, 62.2, 14.7. IR (Diamond-ATR, neat) νmax (cm-1) = 1669, 1635, 1600, 1551, 1498, 1420, 1383, 1256, 1230, 1170, 1035, 764, 631. m.p.: 214 – 216 °C (EtOH). Anal. Calcd for C36H33LaN6O9 ∙ 3 EtOH ∙ 4 La2O3: C, 22.50; H, 2.29; N, 3.75. Found: C, 22.50; H, 1.95; N, 3.45.

Member of collection / collaboration

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

Members

DOI	Description
10.14469/hpc/11548	IR data for Compound 62.
10.14469/hpc/11549	NMR Data for Compound 62.
10.14469/hpc/11430	Primary crystal structure data for Compound 62. Bis(aqua) tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)lanthanum

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