palladium dihydroxide

1: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 2: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 3: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: 75 percent / Ag2CO3/Celite / benzene / 0.17 h / Heating 2: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 3: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 4: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 2: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 2: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 3: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: 95 percent / 3 N HCl / tetrahydrofuran / 5 h / Heating 2: 75 percent / Ag2CO3/Celite / benzene / 0.17 h / Heating 3: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 4: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 5: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: O2, 5,10,15,20-tetraphenylporphine / CH2Cl2 / 0.33 h / Irradiation 2: Me2S / CH2Cl2 / 0.75 h / Ambient temperature 3: 82 percent / NaBH4, H2O, 2 N KOH / tetrahydrofuran; H2O / 4 h / Ambient temperature 4: 95 percent / 3 N HCl / tetrahydrofuran / 5 h / Heating 5: 75 percent / Ag2CO3/Celite / benzene / 0.17 h / Heating 6: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 7: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 8: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

1: 85 percent / SOCl2 / pyridine / 1.) 30 min, ice-bath; 2.) 30 min, r. t. 2: O2, 5,10,15,20-tetraphenylporphine / CH2Cl2 / 0.33 h / Irradiation 3: Me2S / CH2Cl2 / 0.75 h / Ambient temperature 4: 82 percent / NaBH4, H2O, 2 N KOH / tetrahydrofuran; H2O / 4 h / Ambient temperature 5: 95 percent / 3 N HCl / tetrahydrofuran / 5 h / Heating 6: 75 percent / Ag2CO3/Celite / benzene / 0.17 h / Heating 7: 1.) Et3N; 2.) DBN / 1.) CH2Cl2, in ice-bath, 30 min; 2.) benzene, reflux, 1 h 8: 1.) NBS, 1percent HClO4; 2.) AcONa / 2.) Raney-Ni / 1.) acetone, H2O, r. t., 30 min; 2.) MeOH, CH2Cl2, 30 min 9: 70 percent / H2 / Pd(OH)2/C / benzene; ethanol; cyclohexane / 2 h / Heating View Scheme

暂无反应条件数据

1: 0.125 g / pyridine / 6 h / Heating 2: 1.) triethylamine, 2.) isobutyl chloroformate View Scheme