2,2'-azo-bisisobutyronitrile in benzene T=100°C; 0.166667 h; Title compound not separated from byproducts;

aluminum oxide; lithium perchlorate; benzoic acid; acetonitrile in acetonitrile 2 h; constant current electrolysis: 100 mA, graphite cell, platine anode;

NH3 in ammonia NH3 (liquid); inert atmosphere;

in dichloromethane n-Bu3P added to a soln. of the V compound in CH2Cl2 under N2; after 1 h the red soln. is evapd. to dryness; residue extd. with hexane; soln. concd. to a small volume and cooled to -78°C; ppt. filtrated, washed with cold hexane, and sublimed at 150° (0.03 Torr); sublimate recrystd. from hexane (-78°C); elem. anal.;

sulfur in toluene Heating;

in dichloromethane neat (n-Bu)3P is added to a soln. of (C5H5)2V2S4 in CH2Cl2 at room temp. under N2; after 30 min, the reaction mixt. is evapd. to dryness; residue washed with hexane and extd. with CH2Cl2 to remove (Cp)5V5S6; remaining black solid is extd. with CH2Cl2 for 24 h; remainder is (Cp)4V4S4; brown ext. cooled to 0°C to crystallize further (Cp)4V4S4; elem. anal.;

in benzene 0.25 h; Ambient temperatureIrradiation; Title compound not separated from byproducts;

in dichloromethane T=-78°C;

1: tributylphosphine; dimethyl acetylenedicarboxylate in dichloromethane T=0°C; 1 h; 2: carbon disulfide in dichloromethane T=20°C; 20 h;

in dichloromethane a soln. of (Cp)2V2S4 in CH2Cl2 is added to a soln. of (CH3C5H4)2V2S4 in CH2Cl2; a soln. of (n-Bu)3P is added, the resulting mixt. stirred for 1 h at room temp.; 1 further product formed; solvent removed in vac., residue extd. with hexane; ext. concd. to give a black microcrystalline solid; products not further sepd.;