DOI: 10.14469/hpc/11398 Metadata

Created: 2022-10-12 09:54

Last modified: 2024-11-22 09:44

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Crystal structure and NMR and IR Data for ((4-(Ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)zinc polymer (49): Zn(OAc)2•(75.0 mg, 0.344 mmol, 1.00 equiv) was added with stirring to pyrazolone 8 (190 mg, 0.688 mmol, 2.00 equiv) in (10 mL) at 79 °C. After 14 h at reflux, the mixture was cooled to room temperature and placed in an ice-bath. The resultant precipitate was collected by filtration, washed with Et2O (5.0 mL) and dried in vacuo. Zn-pyrazolone complex 49 (191 mg, 0.310 mmol, 90%) 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 49. 1H-NMR (400 MHz, OS(CD3)2): δ (ppm) = 7.33 (s, 1H), 7.10 (d, J = 8.1 Hz, 2H), 6.76 (d, J = 8.1 Hz, 2H), 4.84 (s, 2H), 4.02 (q, J = 7.1 Hz, 2H), 3.68 (s, 3H), 1.11 (t, J = 7.1 Hz, 3H). 13C{1H}-NMR (101 MHz, OS(CD3)2): δ (ppm) = 167.5, 164.6, 158.2, 137.2, 130.8, 128.6, 113.5, 90.5, 59.0, 55.0, 46.9, 14.4. IR (Diamond-ATR, neat) νmax (cm-1) = 1640, 1561, 1526, 1511, 1435, 1359, 1332, 1284, 1238, 1219, 1187, 1172, 1111, 1029, 1003, 869, 801, 779. HRMS (ES-ToF) m/z: [M + H]+ calc. for (C28H31N4O8Zn)+: 615.1428, found: 615.1422. m.p.: 226 – 228 °C (EtOH). Anal. Calcd for C28H30ZnN4O8: C, 54.60; H, 4.91; N, 9.10. Found: C, 54.69; H, 4.91; N, 8.85.

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/11656	NMR Data for Compound 49.
10.14469/hpc/11655	IR Data for Compound 49.
10.14469/hpc/11419	Primary crystal structure data for sample Compound 49. ((4-(Ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)zinc polymer

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