DOI: 10.14469/hpc/11362 Metadata

Created: 2022-10-10 10:09

Last modified: 2024-06-25 09:18

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Crystal structure, NMR and IR data for Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)yttrium (28): YCl3•6H2O (88.0 mg, 0.291 mmol, 1.00 equiv) was added with stirring to pyrazolone 6 (203 mg, 0.874 mmol, 3.00 equiv) in EtOH (4.0 mL) at 79 °C. Aqueous NaOH (2 M; 0.44 mL, 0.874 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 18 h, cooled to room temperature and the precipitate was collected by filtration and dried in vacuo. Y-pyrazolone complex 28 (131 mg, 0.167 mmol, 58%) 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 complex 28. 1H-NMR (400 MHz, (CD3)2CO): δ (ppm) = 8.12 – 8.05 (m, 2H), 7.59 (s, 1H), 7.25 (t, J = 7.9 Hz, 2H), 7.12 – 7.04 (m, 1H), 4.24 (q, J = 7.1 Hz, 2H), 3.83 (s, 1H), 1.24 (t, J = 7.1 Hz, 3H). 13C{1H}-NMR (101 MHz, (CD3)2CO): δ (ppm) = 169.2, 165.7, 141.0, 139.4, 129.2, 125.0, 120.2, 94.4, 61.1, 14.9. IR (Diamond-ATR, neat) νmax (cm-1) = 1641, 1597, 1554, 1528, 1498, 1457, 1429, 1359, 1334, 1237, 1211, 1118, 1083, 951, 784, 752. HRMS (ESI) m/z: [M + H]+ calc. for (C36H34N6O9Y)+: 783.1440, found: 783.1442. m.p.: 148 – 150 °C (EtOH); 175 – 177 °C (EtOH); >200 °C (decomp.). Anal. Calcd for C40H45N6O11Y: C, 54.92; H, 5.19; N, 9.61. Found: C, 53.23; H, 4.93; N, 9.30.

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/11594	NMR Data for Compound 28.
10.14469/hpc/11593	IR Spectrum for Compound 28.
10.14469/hpc/11363	Crystal data for Compound 28. Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)yttrium

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