Reaktionsgleichung
C([O-])(=O)C.[Ni+2:5].C([O-])(=O)C.[CH2:10]([C:12]1[C:32]2[N:33]=[C:14]([CH:15]=[C:16]3[NH:43][C:19](=[CH:20][C:21]4[C:22]([CH2:41][CH3:42])=[C:23]([CH2:39][CH3:40])[C:24]([N:38]=4)=[CH:25][C:26]4[NH:30][C:29]([CH:31]=2)=[C:28]([CH2:34][CH3:35])[C:27]=4[CH2:36][CH3:37])[C:18]([CH2:44][CH3:45])=[C:17]3[CH2:46][CH3:47])[C:13]=1[CH2:48][CH3:49])[CH3:11]>>[Ni:5].[CH2:39]([C:23]1[C:24]2[N:38]=[C:21]([CH:20]=[C:19]3[NH:43][C:16](=[CH:15][C:14]4[C:13]([CH2:48][CH3:49])=[C:12]([CH2:10][CH3:11])[C:32]([N:33]=4)=[CH:31][C:29]4[NH:30][C:26]([CH:25]=2)=[C:27]([CH2:36][CH3:37])[C:28]=4[CH2:34][CH3:35])[C:17]([CH2:46][CH3:47])=[C:18]3[CH2:44][CH3:45])[C:22]=1[CH2:41][CH3:42])[CH3:40]Komponenten
3
Versuchsvorschrift
The nickel acetate is added to the octaethylporphyrin solution; the mixture which results is refluxed for about 24 hours until the electronic spectrum of the reaction mixture indicates that chelation is complete. The reaction mixture is then concentrated to 7 mL and allowed to cool to room temperature of about 22°. Product which precipitates is recovered by filtration, dissolved in a mixed solvent composed of 5 mL dichloromethane and 2 mL methanol, and recrystallized, yielding Ni octaethylporphyrin.
Aufarbeitung
- customthe mixture which results
- temperatureis refluxed for about 24 hours until the electronic spectrum of the reaction mixture
- concentrationThe reaction mixture is then concentrated to 7 mL
- customProduct which precipitates
- filtrationis recovered by filtration
- dissolutiondissolved in a mixed solvent
- customrecrystallized
Quellen und Nachweise
- ORD-Eintrag
- ord-813b69f14299474f9736d8b2058a4e23
- Quelldatensatz
- uspto-grants-1995_06
- Patentnummer
- US05424305
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