(αS,γS,δS,ζS)-N-(3-氨基-2,2-二甲基-3-氧代丙基)-δ-叠氮-γ-羟基-4-甲氧基-3-(3-甲氧基丙氧基)-α, ζ-二异丙基-苯辛酰胺合成路线 （共 55 条）
反应条件
1.1: water; lithium hydroxide hydrate / tetrahydrofuran; methanol / 26 h / 65 - 70 °C 1.2: 0.5 h / 0 - 5 °C 2.1: hydrogenchloride / anhydrous dichloroethane; water / 0 - 5 °C / pH 2.5 2.2: 14.25 h / 0 - 30 °C 3.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 1.25 h / 0 - 5 °C 4.1: sodium azide / ethylene glycol / 20 h / 80 - 85 °C 5.1: triethylamine; 2-hydroxy-pyridine / 16 h / 85 - 90 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; RAMA SUBBA REDDY, Karamala; SAHADEVA REDDY, Maramreddy
Patent: WO2011/148392 A1, 2011 ;
反应条件
1.1: potassium hydroxide; water / 1,4-dioxane / 24 h / Reflux 1.2: 0 - 5 °C 2.1: hydrogenchloride / anhydrous dichloroethane; water / 0 - 5 °C / pH 2.5 2.2: 14.25 h / 0 - 30 °C 3.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 1.25 h / 0 - 5 °C 4.1: sodium azide / ethylene glycol / 20 h / 80 - 85 °C 5.1: triethylamine; 2-hydroxy-pyridine / 16 h / 85 - 90 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; RAMA SUBBA REDDY, Karamala; SAHADEVA REDDY, Maramreddy
Patent: WO2011/148392 A1, 2011 ;
反应条件
1.1: magnesium; ethylene dibromide / tetrahydrofuran / 4.17 h / 63 - 68 °C / Inert atmosphere 1.2: 1 h / 0 - 5 °C 1.3: 0 - 5 °C 2.1: hydrogenchloride / anhydrous dichloroethane; water / 0 - 5 °C / pH 2.5 2.2: 14.25 h / 0 - 30 °C 3.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 1.25 h / 0 - 5 °C 4.1: sodium azide / ethylene glycol / 20 h / 80 - 85 °C 5.1: triethylamine; 2-hydroxy-pyridine / 16 h / 85 - 90 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; RAMA SUBBA REDDY, Karamala; SAHADEVA REDDY, Maramreddy
Patent: WO2011/148392 A1, 2011 ;
反应条件
1.1: hydrogenchloride / anhydrous dichloroethane; water / 0 - 5 °C / pH 2.5 1.2: 14.25 h / 0 - 30 °C 2.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 1.25 h / 0 - 5 °C 3.1: sodium azide / ethylene glycol / 20 h / 80 - 85 °C 4.1: triethylamine; 2-hydroxy-pyridine / 16 h / 85 - 90 °C View Scheme
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; RAMA SUBBA REDDY, Karamala; SAHADEVA REDDY, Maramreddy
Patent: WO2011/148392 A1, 2011 ;
反应条件
1.1: thionyl chloride / 1,2-dichloro-ethane / 5 h / 75 - 80 °C 1.2: 90 - 95 °C 1.3: 10 - 15 °C / pH 14 2.1: triethylamine; 2-hydroxy-pyridine / 30 h / 80 - 90 °C 3.1: sodium hydroxide; dihydrogen peroxide / water / 20 - 40 °C View Scheme
参考文献
MATRIX LABORATORIES LTD; RAMA, Shankar; VADALI, Lakshmana Rao; PALLA, Vijay Kumar; SAIDUGARI, Swamy; MITTAPELLY, Nagaraju; JALDU, Ravikanth; VIJAYA, Krishna Ravi; SESHADRI, Rao Manukonda; DASARL, Srinivasa Rao; SRINIVASA, Rao Potla; DANDALA, Ramesh
Patent: WO2012/52829 A1, 2012 ;
反应条件
1: 2-hydroxy-pyridine; triethylamine / 24 h / 60 - 70 °C 2: sodium hydroxide; dihydrogen peroxide / water; ethanol / 30 - 40 °C View Scheme
参考文献
MAYLAN LABORATORIES LTD; RAMA, Shankar; VADALI, Lakshmana Rao; MITTAPELLY, Nagaraju; RAVI, Vijaya Krishna; SAIDUGARI, Swamy
Patent: WO2013/144979 A1, 2013 ;
反应条件
1.1: tert.-butyl lithium / tetrahydrofuran; pentane / 2 h / -78 °C 1.2: 4 h / -78 °C 2.1: palladium on activated charcoal; hydrogen / methanol / 60 h / 2844.39 Torr 3.1: triethylamine / dichloromethane / 1.17 h / 20 °C 4.1: sodium azide / N,N-dimethyl-formamide / 25 h / 80 °C 5.1: propionic acid / 2 h / 110 °C 6.1: triethylamine / dichloromethane / 0.33 h / 20 °C 7.1: triethylamine / 1,2-dichloro-ethane / 21 h / 80 °C 8.1: water; dihydrogen peroxide; lithium hydroxide hydrate / tetrahydrofuran / 144 h / 55 °C View Scheme
参考文献
Kim, Ji Hei; Ko, Soo Y.
Bulletin of the Korean Chemical Society, 2013 , vol. 34, # 12 p. 3777 - 3781
反应条件
1: palladium on activated charcoal; hydrogen / methanol / 60 h / 2844.39 Torr 2: triethylamine / dichloromethane / 1.17 h / 20 °C 3: sodium azide / N,N-dimethyl-formamide / 25 h / 80 °C 4: propionic acid / 2 h / 110 °C 5: triethylamine / dichloromethane / 0.33 h / 20 °C 6: triethylamine / 1,2-dichloro-ethane / 21 h / 80 °C 7: water; dihydrogen peroxide; lithium hydroxide hydrate / tetrahydrofuran / 144 h / 55 °C View Scheme
参考文献
Kim, Ji Hei; Ko, Soo Y.
Bulletin of the Korean Chemical Society, 2013 , vol. 34, # 12 p. 3777 - 3781
反应条件
1: triethylamine / dichloromethane / 1.17 h / 20 °C 2: sodium azide / N,N-dimethyl-formamide / 25 h / 80 °C 3: propionic acid / 2 h / 110 °C 4: triethylamine / dichloromethane / 0.33 h / 20 °C 5: triethylamine / 1,2-dichloro-ethane / 21 h / 80 °C 6: water; dihydrogen peroxide; lithium hydroxide hydrate / tetrahydrofuran / 144 h / 55 °C View Scheme
参考文献
Kim, Ji Hei; Ko, Soo Y.
Bulletin of the Korean Chemical Society, 2013 , vol. 34, # 12 p. 3777 - 3781
反应条件
1: sodium azide / N,N-dimethyl-formamide / 25 h / 80 °C 2: propionic acid / 2 h / 110 °C 3: triethylamine / dichloromethane / 0.33 h / 20 °C 4: triethylamine / 1,2-dichloro-ethane / 21 h / 80 °C 5: water; dihydrogen peroxide; lithium hydroxide hydrate / tetrahydrofuran / 144 h / 55 °C View Scheme
参考文献
Kim, Ji Hei; Ko, Soo Y.
Bulletin of the Korean Chemical Society, 2013 , vol. 34, # 12 p. 3777 - 3781
