Complete recipeSource: Main
Route 1: Other
p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1
Metal precursorsCu(ClO4)2.6H2O (370 mg, 1 mmol) in 15 mL methanol
Linker precursorsHL1 methanolic solution prepared from 2-hydroxy-5-nitrobenzaldehyde and N,N-dimethyl-1,2-ethylenediamine followed by NaBH4 reduction and HCl acidification
SolventsMethanol and water; CH3OH-H2O mixed solvent about 10:1 v/v
AdditivesNaN3 aqueous solution; concentrated HCl used in ligand workup
AtmosphereOpen air for crystallisation; film drying atmosphere not applicable
Temperaturereflux; ligand solution cooled to 0 C during NaBH4 addition
Time1 h ligand reflux; 1 h complex reflux
Oxidant / reductantNaBH4 (210 mg, 6 mmol) for ligand reduction
Work-upAfter complex reflux, filtered; filtrate kept in open air; slow evaporation gave reddish needle crystals.
Scalability contextCaution in main text notes perchlorate and azide salts of metal complexes may be explosive and only small amounts should be prepared.
Show 8 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Cu(ClO4)2.6H2O | 370 mg, 1 mmol | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Linker | HL1 = 2-[(2-dimethylamino-ethylamino)-methyl]-4-nitrophenol | 1 mmol previously prepared methanolic solution | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Other | 2-hydroxy-5-nitrobenzaldehyde | 835.6 mg, 5 mmol | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Other | N,N-dimethyl-1,2-ethylenediamine | 0.55 mL, 5 mmol | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Reductant | sodium borohydride | 210 mg, 6 mmol | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Acid | concentrated HCl | 5 mL | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Additive | NaN3 | 130 mg, 2 mmol · aqueous solution in 5 mL water | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |
| Solvent | methanol | 30 mL for ligand synthesis; 15 mL for Cu salt solution | p002 · 2.2 Synthesis of the ligands; 2.3 Syntheses of the complexes · Scheme 1 |