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: thionyl chloride; N,N-dimethyl-formamide / toluene / 50 - 55 °C 2.1: toluene / 1 h / 0 - 35 °C 3.1: tetrahydrofuran / 4.5 h / 60 - 65 °C 4.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 4.2: 1 h / -70 - -50 °C 5.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: toluene / 1 h / 0 - 35 °C 2.1: tetrahydrofuran / 4.5 h / 60 - 65 °C 3.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 3.2: 1 h / -70 - -50 °C 4.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: iodine; lithium aluminium tetrahydride / tetrahydrofuran / 2.25 h / 0 - 65 °C 2.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 2.2: 1 h / -70 - -50 °C 3.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: potassium carbonate / 60 - 65 °C 2.1: sodium hydroxide / water / 45 - 50 °C 3.1: ethanol / 5.83 h / 0 - 75 °C 4.1: hydrogenchloride / water; toluene / 1 h / 20 - 25 °C 5.1: thionyl chloride; N,N-dimethyl-formamide / toluene / 50 - 55 °C 6.1: toluene / 1 h / 0 - 35 °C 7.1: tetrahydrofuran / 4.5 h / 60 - 65 °C 8.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 8.2: 1 h / -70 - -50 °C 9.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: ethanol / 5.83 h / 0 - 75 °C 2.1: hydrogenchloride / water; toluene / 1 h / 20 - 25 °C 3.1: thionyl chloride; N,N-dimethyl-formamide / toluene / 50 - 55 °C 4.1: toluene / 1 h / 0 - 35 °C 5.1: tetrahydrofuran / 4.5 h / 60 - 65 °C 6.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 6.2: 1 h / -70 - -50 °C 7.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: hydrogenchloride / water; toluene / 1 h / 20 - 25 °C 2.1: thionyl chloride; N,N-dimethyl-formamide / toluene / 50 - 55 °C 3.1: toluene / 1 h / 0 - 35 °C 4.1: tetrahydrofuran / 4.5 h / 60 - 65 °C 5.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 5.2: 1 h / -70 - -50 °C 6.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: iodine; magnesium; ethyl bromide / tetrahydrofuran / 2 h / 60 - 65 °C / |Inert atmosphere 1.2: 1 h / -70 - -50 °C 2.1: thionyl chloride / 0 - 65 °C View Scheme
参考文献
RANBAXY LABORATORIES LIMITED; VERMA, Shyam Sunder; HANDIQUE, Sourav; AHUJA, Seema; SINGH, Kaptan; PRASAD, Mohan; ARORA, Sudershan, Kumar
Patent: WO2013/46135 A1, 2013 ;
反应条件
1.1: sulfuric acid / 120 - 125 °C 2.1: potassium carbonate; sodium iodide / acetone / Reflux 3.1: sodium tetrahydroborate / ethylene glycol dimethyl ether / 0.17 h 3.2: 3 h / 10 °C 4.1: triethylamine / dichloromethane / 12 h / 25 - 30 °C 5.1: acetonitrile / 30 h / 95 - 100 °C / autoclave; Sealed tube 6.1: isopropyl alcohol / 15 h / 25 - 86 °C 7.1: sodium hydroxide / water 8.1: ethyl bromide; iodine; magnesium / tetrahydrofuran / 1 h / 55 °C / Reflux 8.2: 1 h / -65 - -60 °C 9.1: thionyl chloride / 10 °C / Reflux View Scheme
参考文献
ACTAVIS GROUP PTC EHF
Patent: US2011/124903 A1, 2011 ;
反应条件
1.1: sodium hydroxide / water 2.1: ethyl bromide; iodine; magnesium / tetrahydrofuran / 1 h / 55 °C / Reflux 2.2: 1 h / -65 - -60 °C 3.1: thionyl chloride / 10 °C / Reflux View Scheme
参考文献
ACTAVIS GROUP PTC EHF
Patent: US2011/124903 A1, 2011 ;
反应条件
1: ammonia / water / pH 8 - 9 2: sulfuric acid / 20 °C / Reflux View Scheme
参考文献
ORCHID CHEMICALS AND PHARMACEUTICALS LIMITED; REGURI, Buchi, Reddy; UPPARAPALLI, Sampath, Kumar; SAHU, Nilam; KRISHNASAMY, Mariappan; GNANI PEER MOHAMED, Syed, Ibrahim; SWAMINATHAN, Susi
Patent: WO2011/145019 A1, 2011 ;