2-氧代-4-噁-1,9-二氮杂螺[5.5]十一烷-9-羧酸 1,1-二甲基乙酯合成路线 （共 4 条）
反应条件
hydrogen; palladium 10 on activated carbon in tetrahydrofuran Inert atmosphere;
参考文献
BOEHRINGER INGELHEIM INTERNATIONAL GMBH; DAHMANN, Georg; FIEGEN, Dennis; FLECK, Martin; HOFFMANN, Matthias; KLICIC, Jasna; EAST, Stephen, Peter; NAPIER, Spencer, Charles, R.; SCOTT, John
Patent: WO2012/101013 A1, 2012 ;
Location in patent: Page/Page column 97; 99 ;
WO 2012/101013 A1
反应条件
1.1: water; methanol / Cooling with ice 1.2: 72 h / 20 °C / Cooling with ice 2.1: sodium hydroxide; water / 80 - 108 °C / Industry scale 2.2: 10 - 23 °C / pH 7 - 8 / Industry scale 3.1: lithium aluminium tetrahydride / tetrahydrofuran / 2 h / 19 - 29 °C / Cooling 3.2: 8 - 56 °C 4.1: dichloromethane; water / 0.58 h / Cooling with ice 5.1: potassium tert-butylate / 1,1-dimethylpropan-1-ol / 0.5 h / 20 °C / Inert atmosphere 6.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran / Inert atmosphere View Scheme
参考文献
BOEHRINGER INGELHEIM INTERNATIONAL GmbH; Dahmann, Georg; Fiegen, Dennis; Fleck, Martin; Hoffmann, Matthias; Klicic, Jasna; East, Stephen Peter; Napier, Spencer Charles R.; Scott, John
Patent: US2013/23502 A1, 2013 ;
反应条件
1.1: lithium aluminium tetrahydride / tetrahydrofuran / 2 h / 19 - 29 °C / Cooling 1.2: 8 - 56 °C 2.1: dichloromethane; water / 0.58 h / Cooling with ice 3.1: potassium tert-butylate / 1,1-dimethylpropan-1-ol / 0.5 h / 20 °C / Inert atmosphere 4.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran / Inert atmosphere View Scheme
参考文献
BOEHRINGER INGELHEIM INTERNATIONAL GmbH; Dahmann, Georg; Fiegen, Dennis; Fleck, Martin; Hoffmann, Matthias; Klicic, Jasna; East, Stephen Peter; Napier, Spencer Charles R.; Scott, John
Patent: US2013/23502 A1, 2013 ;
反应条件
1.1: sodium hydroxide; water / 80 - 108 °C / Industry scale 1.2: 10 - 23 °C / pH 7 - 8 / Industry scale 2.1: lithium aluminium tetrahydride / tetrahydrofuran / 2 h / 19 - 29 °C / Cooling 2.2: 8 - 56 °C 3.1: dichloromethane; water / 0.58 h / Cooling with ice 4.1: potassium tert-butylate / 1,1-dimethylpropan-1-ol / 0.5 h / 20 °C / Inert atmosphere 5.1: hydrogen / palladium 10 on activated carbon / tetrahydrofuran / Inert atmosphere View Scheme
参考文献
BOEHRINGER INGELHEIM INTERNATIONAL GmbH; Dahmann, Georg; Fiegen, Dennis; Fleck, Martin; Hoffmann, Matthias; Klicic, Jasna; East, Stephen Peter; Napier, Spencer Charles R.; Scott, John
Patent: US2013/23502 A1, 2013 ;
