Compound 69: Tris((4-(ethoxycarbonyl)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)ytterbium

DOI: 10.14469/hpc/11745 Metadata

Created: 2022-11-08 06:39

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)-1-(4-methoxybenzyl)-1H-pyrazol-5-yl)oxy)ytterbium (69): Yb(OTf)3 (138 mg, 0.223 mmol, 1.00 equiv) was added with stirring to pyrazolone 8 (185 mg, 0.670 mmol, 3.00 equiv) in EtOH (4.0 mL). Aqueous NaOH (2 M; 0.33 mL, 0.670 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 48 h, after which the mixture was cooled to room temperature, H2O (20 mL) was added, and the resultant precipitate was collected by filtration, washed with H2O (3 x 10 mL) and dried in vacuo. Yb-pyrazolone complex 69 (174 mg, 0.174 mmol, 78%) was obtained as a white solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 69. IR (Diamond-ATR, neat) νmax (cm-1) = 1646, 1560, 1523, 1511, 1419, 1247, 1231, 1216, 1172, 1034, 785, 633. HRMS (ES-ToF) m/z: [M – Sol + H]+ calc. for (C42H46N6O12Yb)+: 1000.2557, found: 1000.2607. m.p.: 232 - 234 °C (EtOH) (decomp.). Anal. Calcd for C42H45N6O12Yb ∙ 2 EtOH ∙ Yb2O3: C, 37.20; H, 3.87; N, 5.66. Found: C, 37.21; H, 3.18; N, 5.66.

Files

FilenameSizeTypeDescription
69.cdxml 15KB chemical/x-cdxml Chemdraw connection table
69.png 75KB image/png Image representation
69.mol 5KB 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/3C14H16N2O4.Yb/c3*1-3-20-14(18)12-8-15-16(13(12)17)9-10-4-6-11(19-2)7-5-10;/h3*4-8,17H,3,9H2,1-2H3;/q;;;+3/p-3
inchikey DJEHUAXIYVIHIT-UHFFFAOYSA-K

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