ammonia in methanol; dichloromethane addn. of MeOH satd. with NH3 and nickel acetate to a soln. of octaethylporphyrin N-oxide in CH2Cl2, refluxing under Ar for 24 h; cooling, evapn. in vac., dissolving in CH2Cl2, washing (aq. NH3, H2O), concg. in vac., column chromy. (silica gel, hexane/CH2Cl2) gives a pink fraction of Ni-octaethylporphyrin, elution with CH2Cl2, evapn. in vac., recrystn. (CH2Cl2/MeOH), elem. anal.;

in acetic anhydride; acetic acid Adler, A.D.; Longo, F.R.; Kampas, F.; Kim,J. J. Inorg. Nucl. Chem. 1970, 32, 2443; Bonnett, R.; Dimsdale, M. J. J. Chem. Soc. Perkins Trans. 1972, 2540; OEP added by soxhlet extn. to soln. of (MeCO)2O, MeCO2H and NiCl2 under flow N2; crystals filtered after 12 h, dissolved in boiling C6H6, filtered hot, slowly cooled to room temp. ( 3 d);

in dichloromethane; acetic acid boiling 30 min; chromatography on silica gel with methylene chloride as eluant, crystallisation from methylene chloride and hexane;

in dichloromethane Electrochem. Process; Redn. of Ni(OEP)(1+) at 0.0 V after 10 min at 0.95 V.; Spect. monitored.;

sulfuric acid in N,N-dimethyl-formamide 1 h, 150°C, stirring (2 h); extraction (CH2Cl2), washing (aq NaHCO3, brine), evapn., chromy. (silicagel, hexane-benzene);

sulfuric acid in N,N-dimethyl-formamide addition (1 h, 140°C), stirring (5 h); extraction (CH2Cl2), washing (aq NaHCO3, brine), evapn., chromy. (silicagel, hexane-CH2Cl2);

Electrochem. Process; Repeated oxidn. redn. cycles (0.95 V).; Spect. monitored.;

sulfuric acid in N,N-dimethyl-formamide addition (1 h, 150°C), stirring (2 h); extraction (CH2Cl2), washing (aq NaHCO3, brine), evapn., chromy. (silicagel, hexane-CH2Cl2); anal. H(1) NMR;

Electrochem. Process; Redn. of Ni(OEP)(2+) at 0.0 V after 6-10 min at 1.90 V.; Spect. monitored.;