Compound 18: Bis(ethanol) bis(4-(ethoxycarbonyl)-1H-pyrazol-5-olate)magnesium
DOI: 10.14469/hpc/11339 Metadata
Created: 2022-10-09 11:03
Last modified: 2024-06-27 16:11
License: Creative Commons: Public Domain Dedication 1.0
Funding: (none given)
Description
1H and 13C primary NMR and crystal data forBis(ethanol) bis(4-(ethoxycarbonyl)-1H-pyrazol-5-olate)magnesium (18): MgCl2 (86.0 mg, 0.900 mmol, 1.00 equiv) in H2O and EtOH (1 : 2; 3.0 mL) was added with stirring to pyrazolone 5 (281 mg, 1.80 mmol, 2.00 equiv) in EtOH (3.0 mL) at 79 °C. Aqueous NaOH (2 M; 0.90 mL, 1.80 mmol, 2.00 equiv) was added with stirring and the mixture was heated at reflux for 16 h, cooled to room temperature and the precipitate was collected by filtration and dried in vacuo. Mg-pyrazolone complex 18 (249 mg, 0.584 mmol, 65%) 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 18. 1H-NMR (400 MHz, OS(CD3)2): δ (ppm) = 10.96 (s, 1H), 7.25 (s, 1H), 4.08 (q, J = 7.1 Hz, 2H), 3.35 (s, 4H), 1.17 (t, J = 7.1 Hz, 3H). 13C{1H}-NMR (101 MHz, OS(CD3)2): δ (ppm) = 167.7, 167.5, 137.9, 90.3, 58.8, 14.5. IR (Diamond-ATR, neat) νmax (cm-1) = 3384, 1648, 1571, 1523, 1511, 1431, 1394, 1327, 1281, 1139, 1115, 1015, 921, 788 762, 648. m.p.: 269 – 274 °C (EtOH) (decomp.). Anal. Calcd for C12H14MgN4O6 ∙ 2 H2O: C, 38.89; H, 4.9; N, 15.12. Found: C, 38.8; H, 4.49; N, 14.72.
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/11515 | NMR Data for Compound 18. |
| 10.14469/hpc/11516 | IR data for Compound 18. |
| 10.14469/hpc/11344 | Crystal structure data for compound 18 Bis(ethanol) bis(4-(ethoxycarbonyl)-1-phenyl-1H-pyrazol-5-olate)magnesium |