3-chloro-benzenecarboperoxoic acid in dichloromethane T=25°C; 2 h;

sulfur; CF3CO3H in dichloromethane

1: 92 percent / LiAlH4 / diethyl ether / 1a.) -20 deg C, 0.5 h, b.) from -20 deg C to RT, 1 h 2: 76 percent / PBr3, pyridine / diethyl ether / 1 h / Heating 3: 1.) aq. Na2S2O3, 2.) I2 / 1.) THF, reflux, 1.5 h, 2.) reflux, 1 h 4: 89 percent / m-chloroperoxybenzoic acid / CH2Cl2 / 1 h / 0 - 25 °C View Scheme

1: 96 percent / LiAlH4 / diethyl ether / 0.75 h / -20 °C 2: 92 percent / LiAlH4 / diethyl ether / 1a.) -20 deg C, 0.5 h, b.) from -20 deg C to RT, 1 h 3: 76 percent / PBr3, pyridine / diethyl ether / 1 h / Heating 4: 1.) aq. Na2S2O3, 2.) I2 / 1.) THF, reflux, 1.5 h, 2.) reflux, 1 h 5: 89 percent / m-chloroperoxybenzoic acid / CH2Cl2 / 1 h / 0 - 25 °C View Scheme

1: 76 percent / PBr3, pyridine / diethyl ether / 1 h / Heating 2: 1.) aq. Na2S2O3, 2.) I2 / 1.) THF, reflux, 1.5 h, 2.) reflux, 1 h 3: 89 percent / m-chloroperoxybenzoic acid / CH2Cl2 / 1 h / 0 - 25 °C View Scheme

1: 51 percent / Ni(dppe)Cl2 / diethyl ether / 25 °C 2: 69 percent / sulfur, NH3(g), pyridine / dimethylformamide / 48 h / 110 °C 3: 94 percent / m-CPBA / CH2Cl2 / 2 h / 25 °C View Scheme

1: 51 percent / Ni(dppe)Cl2 / diethyl ether / 25 °C 2: 69 percent / sulfur, NH3(g), pyridine / dimethylformamide / 48 h / 110 °C 3: 94 percent / m-CPBA / CH2Cl2 / 2 h / 25 °C View Scheme

in tetrahydrofuran Irradiation (UV/VIS); dissolving of the Mn compd., photolysing (Hanovia 450W) for 1.5 h, addn. of the dithiinoxide under N2 and stirring at 25°C for 2 h; rotary evapn., column chromy. (silica gel), elution with CH2Cl2-petroleum ether and recrystn. from CH2Cl2-petroleum ether;

tetrahydrofuran in tetrahydrofuran characterization by spectroscopy and crystallography;

η5-C5Me5Fe(CO)2CH3 T=100°C; 1.5 h;