3-[(1R)-3-[双(1-甲基乙基)氨基]-1-苯基丙基]-4-(苯基甲氧基)苯甲酸甲酯合成路线 (共 24 条)
反应条件
1.1: sulfuric acid / 12 h / 120 - 125 °C 2.1: potassium carbonate; sodium iodide / acetone / 25 - 30 °C 2.2: 5.5 h / 15 °C / Reflux 3.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 4 h / 5 - 10 °C / Inert atmosphere 4.1: 4-(N,N-dimethlyamino)pyridine; triethylamine / dichloromethane / 2 h / 0 - 5 °C 5.1: acetonitrile / 32 h / 95 - 100 °C / autoclave; Inert atmosphere 6.1: isopropyl alcohol / 30 - 55 °C 7.1: sodium hydroxide; water / dichloromethane / 0.25 h / 10 - 20 °C / pH 11.5 7.2: 4 h / 25 - 55 °C / Inert atmosphere 7.3: -70 - -10 °C / Inert atmosphere 8.1: thionyl chloride / 5 h / 40 - 45 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; RAGHURAM, Suraparaju; SEETHA RAMA SARMA, Peri
Patent: WO2012/98560 A2, 2012 ;
WO 2012/098560 A2
反应条件
1: hydrogen / 5 palladium on charcoal / ethyl acetate / 18 h / 25 - 30 °C / 2206.72 - 2942.29 Torr / autoclave 2: diisobutylaluminium hydride / toluene / 1 h / -78 °C / Inert atmosphere 3: hydrogen / 5 palladium on charcoal / methanol / 8 h / 25 - 30 °C / 2206.72 - 2942.29 Torr / autoclave View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; RAGHURAM, Suraparaju; SEETHA RAMA SARMA, Peri
Patent: WO2012/98560 A2, 2012 ;
WO 2012/098560 A2
反应条件
1: lithium aluminium tetrahydride / tetrahydrofuran / 14 h / 25 - 30 °C 2: hydrogen / 5 Pd(II)/C(eggshell) / methanol / 50 - 55 °C View Scheme
参考文献
CADILA HEALTHCARE LIMITED; DWIVEDI, Shriprakash Dhar; PRASAD, Ashok; JAIN, Kuldeep Natwarlal
Patent: WO2012/25941 A2, 2012 ;
反应条件
1.1: lithium aluminium tetrahydride / tetrahydrofuran / 14 h / 25 - 30 °C 2.1: hydrogen / 5 Pd(II)/C(eggshell) / methanol / 50 - 55 °C 3.1: dichloromethane / 1.5 h / 0 - 5 °C 3.2: 1 h / 0 - 5 °C View Scheme