ammonia in dichloromethane

in tetrahydrofuran T=25°C; P=760.051 Torr;

in toluene 3 h; Reflux;

zinc in 2-methoxy-ethanol; water (N2 or Ar); mixt. of Ir complex, dppa and acid-washed Zn satd. with CO and pressurized to 4 atm; stirred at 90°C for 45 min; cooled, filtered under nitrogen, concd., chromd. on Florisil with petroleum ether-CH2Cl2 (5:1); recrystd. from THF-hexane; elem. anal.;

trimethylamine N-oxide in hexane under Ar; diphosphine (1 equiv.) and Me3NO (2 equiv.) added to soln. of Co complex in hexane; stirred at 45°C for 5 d; solvent removed under vac.; purified by column chromy. (silica gel, hexane-CH2Cl2 3:1); satisfactory elem. anal.;

1: peroxide 2: S8 View Scheme

tetrachloromethane; ammonia