(2R,3R)-3-(3-甲氧基苯基)-N,N,2-三甲基戊胺合成路线 （共 50 条）
反应条件
1.1: hydrogenchloride / water; tert-butyl methyl ether / 0.5 h / 20 - 25 °C 2.1: thionyl chloride / toluene / 3 h / 75 - 80 °C 3.1: sodium carbonate / toluene; water / 1 h / 0 - 5 °C 4.1: dimethylsulfide borane complex / tetrahydrofuran / 3 h / 20 - 80 °C / Inert atmosphere 4.2: 0.5 h / 0 - 5 °C View Scheme
反应条件
1.1: phosphorus tribromide / 0 - 25 °C 2.1: sodium hydride / dimethyl sulfoxide / 1 h / 25 °C 2.2: 5 h 3.1: sodium hydroxide; ethylene glycol / 4 h / 170 - 180 °C 3.2: pH 1 4.1: di-isopropyl ether / 6 h / 20 - 75 °C 5.1: hydrogenchloride / water; tert-butyl methyl ether / 0.5 h / 20 - 25 °C 6.1: BH3*S(CH3)2 / tetrahydrofuran / 1 h / 50 - 55 °C / Inert atmosphere 6.2: 0 - 5 °C 7.1: triethylamine / 4-(N,N-dimethlyamino)pyridine / dichloromethane / 6 h / 25 - 30 °C 8.1: sodium hydroxide / dimethyl sulfoxide / 0.17 h / 20 - 25 °C 8.2: 2 h / 50 - 55 °C View Scheme
反应条件
1.1: iodine; magnesium / tetrahydrofuran / 1 h / 68 - 75 °C / Inert atmosphere; Reflux 1.2: 12 h / 25 - 30 °C 2.1: sulfuric acid / cyclohexane; tetrahydrofuran / 3 h / 25 - 80 °C 2.2: pH 8 - 9 3.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran / 25 - 30 °C / in an autoclave; Inert atmosphere 3.2: 0 - 5 °C / pH 9 - 10 View Scheme
反应条件
hydrogen; palladium on activated carbon in ethanol T=25°C; P=750.075 - 3750.38 Torr; Product distribution / selectivity;
参考文献
WO2004/108658 A1, ;
Page/Page column 53-55 ;
反应条件
1.1: sodium hydroxide; ethylene glycol / 4 h / 180 °C 1.2: pH 1 2.1: di-isopropyl ether / 6 h / 20 - 75 °C 3.1: hydrogenchloride / water; tert-butyl methyl ether / 0.5 h / 20 - 25 °C 4.1: BH3*S(CH3)2 / tetrahydrofuran / 1 h / 50 - 55 °C / Inert atmosphere 4.2: 0 - 5 °C 5.1: triethylamine / 4-(N,N-dimethlyamino)pyridine / dichloromethane / 6 h / 25 - 30 °C 6.1: sodium hydroxide / dimethyl sulfoxide / 0.17 h / 20 - 25 °C 6.2: 2 h / 50 - 55 °C View Scheme
反应条件
1.1: sodium hydroxide; ethylene glycol / 4 h / 170 - 180 °C 1.2: pH 1 2.1: di-isopropyl ether / 6 h / 20 - 75 °C 3.1: hydrogenchloride / water; tert-butyl methyl ether / 0.5 h / 20 - 25 °C 4.1: BH3*S(CH3)2 / tetrahydrofuran / 1 h / 50 - 55 °C / Inert atmosphere 4.2: 0 - 5 °C 5.1: triethylamine / 4-(N,N-dimethlyamino)pyridine / dichloromethane / 6 h / 25 - 30 °C 6.1: sodium hydroxide / dimethyl sulfoxide / 0.17 h / 20 - 25 °C 6.2: 2 h / 50 - 55 °C View Scheme
反应条件
1.1: sodium hydroxide; ethylene glycol / 4 h / 170 - 180 °C 1.2: pH 1 2.1: di-isopropyl ether / 6 h / 20 - 75 °C 3.1: hydrogenchloride / water; tert-butyl methyl ether / 0.5 h / 20 - 25 °C 4.1: BH3*S(CH3)2 / tetrahydrofuran / 1 h / 50 - 55 °C / Inert atmosphere 4.2: 0 - 5 °C 5.1: triethylamine / 4-(N,N-dimethlyamino)pyridine / dichloromethane / 6 h / 25 - 30 °C 6.1: sodium hydroxide / dimethyl sulfoxide / 0.17 h / 20 - 25 °C 6.2: 2 h / 50 - 55 °C View Scheme
反应条件
1.1: triethylamine; lithium hexamethyldisilazane / toluene / 2.83 h / -60 °C / Inert atmosphere 1.2: 0.17 h 1.3: Cooling with ice 2.1: hydrogen / 5 palladium on charcoal / methanol / 18 h / 20 °C / 3000.3 Torr 3.1: thionyl chloride / toluene / 4 h / 90 °C 4.1: triethylamine / dichloromethane / 0.83 h / 20 °C / Cooling with ice 5.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 1 h / Inert atmosphere; Reflux 5.2: 0.5 h / 20 °C / Cooling with ice View Scheme
反应条件
1.1: hydrogenchloride / ethyl acetate; water / 0.25 h / 20 °C 2.1: thionyl chloride / toluene / 4 h / 90 °C 3.1: triethylamine / dichloromethane / 1 h / 20 °C / Cooling with ice 4.1: hydrogen / 5 palladium on charcoal / methanol / 16 h / 20 °C / 3375.34 Torr / Inert atmosphere 5.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 1 h / Inert atmosphere; Reflux 5.2: 0.5 h / 20 °C / Cooling with ice View Scheme
反应条件
1.1: thionyl chloride / toluene / 4 h / 90 °C 2.1: triethylamine / dichloromethane / 1 h / 20 °C / Cooling with ice 3.1: hydrogen / 5 palladium on charcoal / methanol / 16 h / 20 °C / 3375.34 Torr / Inert atmosphere 4.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 1 h / Inert atmosphere; Reflux 4.2: 0.5 h / 20 °C / Cooling with ice View Scheme
