diethyl ether; sulfur

sulfur in acetone Schlenk technique (N2): suspn. of Fe6S6(PEt3)4Cl2, sulfur and (Me4N)Cl in acetone stirred (overnight); ether added to filtrate, -20 ° C (overnight), solid collected, washed (ether), Et3PS (filtrate) detected by 31P NMR;

NH3 in ammonia NH3 (liquid); inert atmosphere;

in dichloromethane T=-78°C;

sulfur in acetone Schlenk technique (N2): suspn. of Fe6S6(PEt3)4Cl2, sulfur and {(Ph3P)2N}Cl in acetone stirred (overnight), brown solid filtered (filtrate contained Et3PS and slight amount of Et3PO); washed (acetone), treated with acetonitrile, filtered, ether added to filtrate, -20 ° C (overnight), filtered, residue from MeCN treatment taken up in DMF, S removed, ether added (filtrate), -20 °C (overnight), 31P NMR, UV/Vis;

1: POCl3 / benzene 2: Bu3EtN(1+)*I(1-); PSCl3 / benzene View Scheme

tetraphosphorus decasulfide

ethanol; silver(l) oxide beim Erhitzen mit Wasser auf 100grad;

air

toluene