(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
5 palladium on charcoal; hydrogen in ethanol T=24°C; P=3750.38 Torr; 22 h;
参考文献
Siegfried AG; Cyr, Patrick; Crump, Roger; Sahli, Stefan; Blum, Vinzenz
Patent: EP2674414 A1, 2013 ;
Location in patent: Paragraph 0090; 0091; 0092 ;
反应条件
lithium aluminium tetrahydride in tetrahydrofuran 2 h; Cooling with ice;
参考文献
Zhang, Qiang; Zhang, Rongxia; Tian, Guanghui; Li, Jianfeng; Zhu, Fuqiang; Jiang, Xiangrui; Shen, Jingshan
Patent: US2014/46074 A1, 2014 ;
Location in patent: Paragraph 0181-0182 ;
反应条件
1: With methanesulfonic acid; sulfuric acid in tetrahydrofuran; cyclohexane T=25 - 78°C; 3 h; 2: With palladium 10 on activated carbon; hydrogen in tetrahydrofuran; cyclohexane T=25 - 30°C; AutoclaveInert atmosphere;
参考文献
Indoco Remedies Limited; Rajadhyaksha, Mangesh Narayan; Nair, Ranjeet; Deshmukh, Sandip Kacharu; Khabale, Somnath Ambadas; Panandikar, Aditi Milind
Patent: US2013/137890 A1, 2013 ;
Location in patent: Paragraph 0057; 0058; 0059 ;
反应条件
1: dimethylammonium chloride With sodium hydroxide in dimethyl sulfoxide T=20 - 25°C; 0.166667 h; 2: (R),(R)-toluene-4-sulfonic acid 3-(3-methoxy-phenyl)-2-methyl-pentyl ester in dimethyl sulfoxide T=50 - 55°C; 2 h;
参考文献
IND-SWIFT LABORATORIES LIMITED; BHIRUD, Shekhar Bhaskar; JOHAR, Perminder Singh; SHARMA, Ekta; JAMSHAD, Danish; PRAJAPATY, Ramkaran
Patent: WO2011/92719 A2, 2011 ;
Location in patent: Page/Page column 43 ;
反应条件
1: With hydrogen; palladium 10 on activated carbon in tetrahydrofuran T=25 - 30°C; in an autoclaveInert atmosphere; 2: With sodium hydroxide in water T=0 - 5°C; pH=9 - 10; Product distribution / selectivity;
参考文献
Indoco Remedies Limited; Rajadhyaksha, Mangesh Narayan; Nair, Ranjeet; Deshmukh, Sandip Kacharu; Khabale, Somnath Ambadas; Panandikar, Aditi Milind
Patent: US2013/137890 A1, 2013 ;
Location in patent: Paragraph 0054; 0055; 0056 ;
反应条件
methanesulfonic acid; hydrogen; bis(norbornadiene)rhodium(I) tetrafluoroborate; (S)-Solphos in ethanol T=0 - 25°C; P=7500.75 - 15001.5 Torr; 16.5 - 67.5 h; Product distribution / selectivity;
参考文献
US2009/43132 A1, ;
Page/Page column 10-12 ;
反应条件
lithium aluminium tetrahydride in tetrahydrofuran T=20 - 70°C; 12 h; Inert atmosphereReflux;
参考文献
WO2012/146978 A2, ;
Page/Page column 20-21 ;
反应条件
1.1: thionyl chloride / toluene / 3 h / 75 - 80 °C 2.1: sodium carbonate / toluene; water / 1 h / 0 - 5 °C 3.1: dimethylsulfide borane complex / tetrahydrofuran / 3 h / 20 - 80 °C / Inert atmosphere 3.2: 0.5 h / 0 - 5 °C View Scheme
反应条件
1.1: sodium carbonate / toluene; water / 1 h / 0 - 5 °C 2.1: dimethylsulfide borane complex / tetrahydrofuran / 3 h / 20 - 80 °C / Inert atmosphere 2.2: 0.5 h / 0 - 5 °C View Scheme
反应条件
1.1: carbon tetrabromide / 10 h / 60 °C 2.1: triethylamine; lithium hexamethyldisilazane / toluene / 2.83 h / -60 °C / Inert atmosphere 2.2: 0.17 h 2.3: Cooling with ice 3.1: hydrogen / 5 palladium on charcoal / methanol / 18 h / 20 °C / 3000.3 Torr 4.1: thionyl chloride / toluene / 4 h / 90 °C 5.1: triethylamine / dichloromethane / 0.83 h / 20 °C / Cooling with ice 6.1: sodium bis(2-methoxyethoxy)aluminium dihydride / toluene / 1 h / Inert atmosphere; Reflux 6.2: 0.5 h / 20 °C / Cooling with ice View Scheme