Compound 66: Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)dysprosium
DOI: 10.14469/hpc/11409 Metadata
Created: 2022-10-12 10:22
Last modified: 2024-06-25 09:38
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)dysprosium (66): DyCl3•6H2O (101 mg, 0.267 mmol, 1.00 equiv) was added with stirring to pyrazolone 6 (186 mg, 0.801 mmol, 3.00 equiv) in EtOH (4.5 mL) at 79 °C. Aqueous NaOH (2 M; 0.16 mL, 0.801 mmol, 3.00 equiv) was added with stirring and the mixture was heated at reflux for 20 h. H2O was added (20 mL), the mixture was cooled to room temperature, the precipitate was collected by filtration, washed with H2O (3 x 10 mL) and dried in vacuo. Dy-pyrazolone complex 66 (115 mg, 0.134 mmol, 50%) was obtained as an off-white solid. Crystals suitable for X-ray crystallography were obtained by slow evaporation from an EtOH solution of complex 66. Repeating the reaction with Dy(OTf)3 (195 mg, 0.320 mmol, 1.00 equiv), pyrazolone 6 (223 mg, 0.960 mmol, 3.00 equiv) and aqueous NaOH (2M, 0.48 mL, 0.960 mmol, 3.00 equiv) according to the above procedure resulted in an improved yield of Dy-pyrazolone complex 66 (237 mg, 0.277 mmol, 87%). IR (Diamond-ATR, neat) νmax (cm-1) = 1636, 1596, 1552, 1528, 1497, 1429, 1359, 1333, 1237, 1211, 1118, 1082, 1060, 951, 782, 747. m.p.: 148 – 150 °C (EtOH); >250 °C (decomp.). Anal. Calcd for C36H39N6O12Dy: C, 47.50; H, 4.32; N, 9.23. Found: C, 47.23; H, 4.28; N, 7.80.
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/11493 | IR data for Compound 66 |
| 10.14469/hpc/11436 | Primary crystal structure data for Compound 66. Tris((4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-yl)oxy)dysprosium |