5-叔丁基-2,3-二氢-1H-茚-1-胺合成路线 (共 8 条)
反应条件
ammonia; hydrogen; palladium 10 on activated carbon in methanol; water
T=50°C; P=3102.97 Torr; 16 h;
参考文献
Gomtsyan, Arthur; Bayburt, Erol K.; Koenig, John R.; Lee, Chih-Hung
Patent: US2004/254188 A1, 2004 ;
Location in patent: Page 14 ;
US 20040254188 A1
反应条件
ammonia; hydrogen; palladium 10 on activated carbon in methanol
P=3102.97 Torr; 6 h;
参考文献
GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; FRORMANN, Sven
Patent: WO2012/62463 A1, 2012 ;
Location in patent: Page/Page column 77 ;
反应条件
1.1: AlCl3, aluminium chloride / dichloromethane / 0.25 h / 0 °C
1.2: 1.25 h / 0 °C
1.3: Cooling with ice
2.1: sulfuric acid / dichloromethane / 2 h / 90 °C
3.1: hydroxylamine hydrochloride; sodium acetate / methanol / 2 h / Reflux
4.1: potassium tert-butylate / tetrahydrofuran / 20 °C
4.2: 0 - 20 °C
5.1: hydrogen; ammonia / palladium 10 on activated carbon / methanol / 6 h / 3102.97 Torr
View Scheme
参考文献
GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; FRORMANN, Sven
Patent: WO2012/62463 A1, 2012 ;
反应条件
1.1: hydroxylamine hydrochloride; sodium acetate / methanol / 2 h / Reflux
2.1: potassium tert-butylate / tetrahydrofuran / 20 °C
2.2: 0 - 20 °C
3.1: hydrogen; ammonia / palladium 10 on activated carbon / methanol / 6 h / 3102.97 Torr
View Scheme
参考文献
GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; FRORMANN, Sven
Patent: WO2012/62463 A1, 2012 ;
反应条件
1.1: sulfuric acid / dichloromethane / 2 h / 90 °C
2.1: hydroxylamine hydrochloride; sodium acetate / methanol / 2 h / Reflux
3.1: potassium tert-butylate / tetrahydrofuran / 20 °C
3.2: 0 - 20 °C
4.1: hydrogen; ammonia / palladium 10 on activated carbon / methanol / 6 h / 3102.97 Torr
View Scheme
参考文献
GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; FRORMANN, Sven
Patent: WO2012/62463 A1, 2012 ;
反应条件
1.1: potassium tert-butylate / tetrahydrofuran / 20 °C
1.2: 0 - 20 °C
2.1: hydrogen; ammonia / palladium 10 on activated carbon / methanol / 6 h / 3102.97 Torr
View Scheme
参考文献
GRUeNENTHAL GMBH; FRANK, Robert; CHRISTOPH, Thomas; FRORMANN, Sven
Patent: WO2012/62463 A1, 2012 ;
反应条件
1: water; methanol / 1 h / 65 °C / |Large scale
2: N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 1 h / 20 °C
3: sodium hydroxide / methanol / 20 °C
View Scheme
参考文献
Lukin, Kirill; Hsu, Margaret C.; Chambournier, Gilles; Kotecki, Brian; Venkatramani; Leanna
Organic Process Research and Development, 2007 , vol. 11, # 3 p. 578 - 584
反应条件
1: With (R)-N-acetylleucine in methanol
T=65°C; 1 h;
2: With sodium hydroxide
参考文献
Gruenenthal GmbH
Patent: US2012/115893 A1, 2012 ;
Location in patent: Page/Page column 31 ;
US 20120115893 A1