N-烯丙基-N-[2-(羟基亚氨基)乙基]氨基甲酸苄酯合成路线 （共 6 条）
反应条件
1: in pentan-1-ol T=135°C; 20 h; Inert atmosphere; 2: With hydrogen; Raney Ni in ethanol; pentan-1-ol P=3102.97 Torr; 4 h;
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50202 A1, 2011 ;
WO 2011/050202 A1
反应条件
1.1: pentan-1-ol / 20 h / 135 °C 2.1: hydrogen / Raney Ni / ethanol; pentan-1-ol / 4 h / 3102.97 Torr 3.1: sodium hydrogencarbonate / ethanol; water; pentan-1-ol / 15 h / 20 °C / Inert atmosphere 4.1: triethylamine / dichloromethane / 0 - 20 °C 5.1: trifluoroacetic acid / dichloromethane / 20 h 5.2: 1.5 h / 60 °C 6.1: ethanol; water / 0.67 h / 20 °C 7.1: hydrogen / 5 Pd(II)/C(eggshell) / methanol / 1.5 h / 775.74 Torr / Inert atmosphere View Scheme
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50202 A1, 2011 ;
WO 2011/050202 A1
反应条件
1: sodium hydroxide / toluene; water / 4 h / 0 - 20 °C / Inert atmosphere
2: potassium hydroxide / N-benzyl-N,N,N-triethylammonium chloride / toluene / 48 h / 50 °C / Inert atmosphere
3: formic acid / 20 °C / Inert atmosphere
4: hydroxylamine hydrochloride; sodium acetate / acetonitrile; water / 20 °C / Inert atmosphere
View Scheme
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50200 A1, 2011 ;
WO 2011/050200 A1
反应条件
1: potassium hydroxide / N-benzyl-N,N,N-triethylammonium chloride / toluene / 48 h / 50 °C / Inert atmosphere
2: formic acid / 20 °C / Inert atmosphere
3: hydroxylamine hydrochloride; sodium acetate / acetonitrile; water / 20 °C / Inert atmosphere
View Scheme
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50200 A1, 2011 ;
WO 2011/050200 A1
反应条件
1: formic acid / 20 °C / Inert atmosphere
2: hydroxylamine hydrochloride; sodium acetate / acetonitrile; water / 20 °C / Inert atmosphere
View Scheme
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50200 A1, 2011 ;
WO 2011/050200 A1
反应条件
1.1: pentan-1-ol / 20 h / 135 °C / Inert atmosphere
1.2: Raney Ni / 4 h / 3102.97 Torr
2.1: sodium hydrogencarbonate / ethanol; water; pentan-1-ol / 15 h / 20 °C / Inert atmosphere
3.1: triethylamine / dichloromethane / 22.33 h / 0 - 20 °C / Inert atmosphere
4.1: trifluoroacetic acid / dichloromethane / 20 h
4.2: pH ~ 12
5.1: sodium hydroxide / ethanol; water / 1.5 h / 60 °C
View Scheme
参考文献
JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.
Patent: WO2011/50202 A1, 2011 ;
WO 2011/050202 A1
