1: sulfuric acid / 24 h / |Reflux; |Inert atmosphere 2: hydrogen; [(D)*Ir(1,4-cyclooctadiene)]+[tetrakis(3,5-bis(trifluoromethyl)phenyl)borate]- / dichloromethane / 15 h / 20 °C / 15001.5 Torr / |Inert atmosphere 3: lithium aluminium tetrahydride / |Inert atmosphere View Scheme

1.1: thionyl chloride 2.1: n-butyllithium / hexane; tetrahydrofuran / 0.25 h / -78 °C 2.2: 0.75 h / -78 - 0 °C 3.1: sodium hexamethyldisilazane / tetrahydrofuran / -78 °C 3.2: 6 h / -50 °C 4.1: lithium borohydride / tetrahydrofuran / 0 °C 5.1: 1H-imidazole / dichloromethane / 20 °C 6.1: diisobutylaluminium hydride / dichloromethane; toluene / 3 h / -40 °C 7.1: triphenylphosphine; carbon tetrabromide / dichloromethane / 0.5 h / 20 °C / |Inert atmosphere 8.1: N,N,N',N,-tetramethylethylenediamine; anhydrous iron chloride / tetrahydrofuran / 0.5 h / 0 °C 9.1: tetrabutyl ammonium fluoride / tetrahydrofuran / 3 h / 20 °C 10.1: 1-hydroxy-3H-benz[d][1,2]iodoxole-1,3-dione / dimethyl sulfoxide / 20 °C 11.1: tetrahydrofuran / 2.25 h / 0 - 20 °C 12.1: pyridine / 20 °C 13.1: potassium tert-butylate / dimethyl sulfoxide / 5 h / 20 °C 14.1: methyl-magnesium iodide / diethyl ether / 0.17 h / 180 °C / |Inert atmosphere View Scheme

sulfuric acid 24 h; RefluxInert atmosphere;

n-butyllithium; diethylamine in tetrahydrofuran; hexane 1.) -78 deg C, 0.5 h, 2.) room temp., 1 h; Yield given. Yields of byproduct given. Title compound not separated from byproducts;

1: thionyl chloride 2: H2O View Scheme

1: 1) O2, tetraphenyl phosphine; 2) conc. H2SO4 / 1) chloroform, -5 degC to 0 degC, irradiation 2: 27 percent / Ph3P / CHCl3 / -40 degC to room temp. View Scheme

diphenyldisulfane in benzene 24 h; Irradiation;

暂无反应条件数据

暂无反应条件数据

1: PCl3 3: MCPBA / CH2Cl2 / 12 h / 35 °C 4: 76 percent / LiAlH4 / tetrahydrofuran / 4 h / Heating View Scheme