6-(4-甲基哌嗪-1-基)-4-(2-甲基苯基)烟酰胺合成路线 （共 13 条）
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
Location in patent: Page/Page column 25 ;
反应条件
1.1: tetrahydrofuran / 19 h / 0 - 20 °C 1.2: acetic acid / tetrahydrofuran / -60 °C 1.3: Mn(OAc)3*2H2O / tetrahydrofuran / 1.5 h / -60 - 20 °C 2.1: SOCl2; DMF / tetrahydrofuran / 2.5 h / 50 °C 3.1: 7.8 g / NH3 / tetrahydrofuran; H2O / 0.5 h / 0 °C 4.1: 2 h / 100 °C View Scheme
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
反应条件
methanesulfonic acid T=100°C; 5 h;
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
反应条件
1.1: tetrahydrofuran / 21 h / 20 - 30 °C 1.2: acetic acid / tetrahydrofuran / 0.25 h 1.3: DDQ / tetrahydrofuran / 1 h / 20 °C 2.1: 4 h / 100 °C 3.1: MeSO3H / 5 h / 100 °C View Scheme
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
反应条件
1: SOCl2; DMF / tetrahydrofuran / 2.5 h / 50 °C 2: 7.8 g / NH3 / tetrahydrofuran; H2O / 0.5 h / 0 °C 3: 2 h / 100 °C View Scheme
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
反应条件
1.1: 66.8 g / toluene / 1.17 h 2.1: tetrahydrofuran / 21 h / 20 - 30 °C 2.2: acetic acid / tetrahydrofuran / 0.25 h 2.3: DDQ / tetrahydrofuran / 1 h / 20 °C 3.1: 4 h / 100 °C 4.1: MeSO3H / 5 h / 100 °C View Scheme
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
反应条件
1.1: tetrahydrofuran / 19 h / 0 - 20 °C 1.2: acetic acid / tetrahydrofuran / -60 °C 1.3: Mn(OAc)3*2H2O / tetrahydrofuran / 1.5 h / -60 - 20 °C 2.1: SOCl2; DMF / tetrahydrofuran / 2.5 h / 50 °C 3.1: 7.8 g / NH3 / tetrahydrofuran; H2O / 0.5 h / 0 °C 4.1: 2 h / 100 °C View Scheme
参考文献
Helsinn Healthcare SA; Fadini, Luca; Manini, Peter; Pietra, Claudio; Giuliano, Claudio; Lovati, Emanuela; Cannella, Roberta; Venturini, Alessio; Stella, Valentino J.
Patent: US8426450 B1, 2013 ;
反应条件
1: methanol / 20.25 h / 18 - 25 °C 2: hydrogen; triethylamine; 20 palladium(II) hydroxide on carbon / methanol / 10 h / 25 °C / 2223.8 - 2497.89 Torr 3: sulfuric acid / toluene / 12 h / 70 °C View Scheme
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
反应条件
1: morpholine / isopropyl alcohol / 1 h / 20 - 33 °C 2: triethylamine / methanol / 66.02 h / 25 °C / |Reflux 3: trichlorophosphate / 10 h / 135 °C 4: methanol / 20.25 h / 18 - 25 °C 5: hydrogen; triethylamine; 20 palladium(II) hydroxide on carbon / methanol / 10 h / 25 °C / 2223.8 - 2497.89 Torr 6: sulfuric acid / toluene / 12 h / 70 °C View Scheme
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
反应条件
1: triethylamine / methanol / 66.02 h / 25 °C / |Reflux 2: trichlorophosphate / 10 h / 135 °C 3: methanol / 20.25 h / 18 - 25 °C 4: hydrogen; triethylamine; 20 palladium(II) hydroxide on carbon / methanol / 10 h / 25 °C / 2223.8 - 2497.89 Torr 5: sulfuric acid / toluene / 12 h / 70 °C View Scheme
参考文献
Harrington, Peter J.; Johnston, Dave; Moorlag, Henk; Wong, Jim-Wah; Hodges, L. Mark; Harris, Les; McEwen, Gerald K.; Smallwood, Blair
Organic Process Research and Development, 2006 , vol. 10, # 6 p. 1157 - 1166
