外消旋5-羟甲基去异丙基托特罗定-d6合成路线 （共 69 条）
反应条件
1.1: hydrogen / 5 palladium on charcoal / methanol / 25 - 50 °C / 10343.2 Torr / Autoclave 2.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 0 - 30 °C / Inert atmosphere 3.1: (+)-(R)-malic acid / isopropyl alcohol; di-isopropyl ether / 20 - 80 °C 3.2: pH 10 View Scheme
反应条件
1.1: 25 - 112 °C / Autoclave 2.1: isopropyl alcohol / 14 h / 25 - 80 °C 3.1: sodium hydroxide / water / 0 - 35 °C / pH 9 4.1: magnesium / iodine / tetrahydrofuran / 1 h / -70 - 70 °C 4.2: -5 - 35 °C 4.3: pH 1 - 2 5.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 0.25 h / 0 - 5 °C 6.1: hydrogen / 5 palladium on charcoal / methanol / 2 h / 25 - 35 °C / Autoclave 6.2: 25 - 35 °C View Scheme
反应条件
1: sulfuric acid; acetic acid / 16 h / 100 °C 2: acetone / 2 h / 25 - 35 °C 3: boron trifluoride diethyl etherate / tetrahydrofuran / 1 h / -20 °C 4: hydrogen / 5 palladium on charcoal / methanol / 18 h / 25 - 35 °C / 2942.29 Torr / autoclave 5: potassium carbonate / acetone / 6 h / Reflux View Scheme
参考文献
WO2012/98560 A2, ;
WO 2012/098560 A2
反应条件
1: acetone / 2 h / 25 - 35 °C 2: boron trifluoride diethyl etherate / tetrahydrofuran / 1 h / -20 °C 3: hydrogen / 5 palladium on charcoal / methanol / 18 h / 25 - 35 °C / 2942.29 Torr / autoclave 4: potassium carbonate / acetone / 6 h / Reflux View Scheme
参考文献
WO2012/98560 A2, ;
WO 2012/098560 A2
反应条件
1: boron trifluoride diethyl etherate / tetrahydrofuran / 1 h / -20 °C 2: hydrogen / 5 palladium on charcoal / methanol / 18 h / 25 - 35 °C / 2942.29 Torr / autoclave 3: potassium carbonate / acetone / 6 h / Reflux View Scheme
参考文献
WO2012/98560 A2, ;
WO 2012/098560 A2
反应条件
1: hydrogen / 5 palladium on charcoal / methanol / 18 h / 25 - 35 °C / 2942.29 Torr / autoclave 2: potassium carbonate / acetone / 6 h / Reflux View Scheme
参考文献
WO2012/98560 A2, ;
WO 2012/098560 A2
反应条件
potassium carbonate in acetone 6 h; Reflux; Product distribution / selectivity;
参考文献
WO2012/98560 A2, ;
Page/Page column 69 ;
WO 2012/098560 A2
反应条件
1.1: potassium carbonate; potassium iodide / toluene; methanol / 20 h / Reflux 2.1: methanesulfonic acid / 3 h / 100 °C 3.1: sodium tetrahydroborate / methanol / 2 h / 0 °C 3.2: 0.08 h 3.3: pH 8 4.1: 1,1-dimethylpropan-1-ol / 25 - 70 °C 5.1: potassium carbonate / toluene; water / 1 h / 50 °C View Scheme
反应条件
1.1: methanesulfonic acid / 3 h / 100 °C 2.1: sodium tetrahydroborate / methanol / 2 h / 0 °C 2.2: 0.08 h 2.3: pH 8 3.1: 1,1-dimethylpropan-1-ol / 25 - 70 °C 4.1: potassium carbonate / toluene; water / 1 h / 50 °C View Scheme
反应条件
1.1: toluene / 21 h / 100 - 110 °C 2.1: tetrabutyl ammonium fluoride / tetrahydrofuran / 2 h / 50 °C 2.2: 0.5 h / 30 °C 3.1: hydrogenchloride; water / ethyl acetate / 1 h / 50 °C 4.1: sodium hydroxide; sodium tetrahydroborate / toluene; methanol / 0.5 h / 0 - 5 °C 5.1: 1,1-dimethylpropan-1-ol / 4 h / 65 - 75 °C / Resolution of racemate 6.1: potassium carbonate / toluene / 2 h / 50 °C View Scheme
