[3-(二甲基氨基)丙基]三苯基磷溴化物氢溴酸盐合成路线 （共 8 条）
反应条件
in ethanol; water T=20 - 100°C; Sealed tube;
参考文献
NEKTAR THERAPEUTICS; RIGGS-SAUTHIER, Jennifer; DENG, Bo-Liang; GURSAHANI, Hema
Patent: WO2012/79017 A1, 2012 ;
Location in patent: Page/Page column 68 ;
WO 2012/079017 A1
反应条件
1: anhydrous 3-(dimethylamino)propyltriphenylphosphonium bromide hydrobromide With sodium hydride in tetrahydrofuran Wittig Reaction; 3 h; Heating / reflux; 2: (11-oxo-6,11-dihydro-dibenzo[b,e]oxepin-2-yl)-acetic acid benzyl ester in tetrahydrofuran T=0 - 30°C; 3 h; 3: With hydrogenchloride; water in di-isopropyl ether pH=2;
参考文献
WO2009/81417 A2, ;
Page/Page column 11-12 ;
反应条件
1: anhydrous 3-(dimethylamino)propyltriphenylphosphonium bromide hydrobromide With sodium hydride in tetrahydrofuran; mineral oil T=65°C; Inert atmosphere; 2: 6,11-dihydro-11-oxo-dibenz[b,e]oxepine-2-acetic acid in tetrahydrofuran; mineral oil T=20°C; Wittig Reaction; 15 h; 3: With hydrogenchloride in tetrahydrofuran; water; mineral oil pH=2.27; Product distribution / selectivity;
参考文献
MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; ESWARAIAH, Sajja; SATYANARAYANA, Komati
Patent: WO2011/128911 A2, 2011 ;
Location in patent: Page/Page column 14 ;
反应条件
sodium carbonate in isopropyl alcohol T=50°C; 6 h; Product distribution / selectivity;
参考文献
US2007/232814 A1, ;
Page/Page column 24 ;
反应条件
1.1: n-BuLi / tetrahydrofuran; hexane / 0.67 h / 0 °C
1.2: tetrahydrofuran; hexane / 60 °C
2.1: 5.15 g / H2 / Rh/C / methanol / 19 h
3.1: n-BuLi / tetrahydrofuran; hexane / 0.17 h / -78 °C
3.2: 71 percent / tetrahydrofuran; hexane / -78 - 20 °C
View Scheme
参考文献
Wuitschik, Georg; Rogers-Evans, Mark; Mueller, Klaus; Fischer, Holger; Wagner, Bjoern; Schuler, Franz; Polonchuk, Liudmila; Carreira, Erick M.
Angewandte Chemie - International Edition, 2006 , vol. 45, # 46 p. 7736 - 7739
反应条件
1.1: n-BuLi / tetrahydrofuran; hexane / 0.67 h / 0 °C
1.2: tetrahydrofuran; hexane / 60 °C
2.1: 5.15 g / H2 / Rh/C / methanol / 19 h
View Scheme
参考文献
Wuitschik, Georg; Rogers-Evans, Mark; Mueller, Klaus; Fischer, Holger; Wagner, Bjoern; Schuler, Franz; Polonchuk, Liudmila; Carreira, Erick M.
Angewandte Chemie - International Edition, 2006 , vol. 45, # 46 p. 7736 - 7739
反应条件
1.1: n-BuLi / tetrahydrofuran; hexane / 0.67 h / 0 °C
1.2: tetrahydrofuran; hexane / 60 °C
2.1: 5.15 g / H2 / Rh/C / methanol / 19 h
3.1: n-BuLi / tetrahydrofuran; hexane; diethyl ether / 0.75 h / -78 °C
3.2: triisopropyl borate / tetrahydrofuran; diethyl ether; hexane / -78 - 20 °C
3.3: aq. HCl / tetrahydrofuran; diethyl ether; hexane / 0.33 h
View Scheme
参考文献
Wuitschik, Georg; Rogers-Evans, Mark; Mueller, Klaus; Fischer, Holger; Wagner, Bjoern; Schuler, Franz; Polonchuk, Liudmila; Carreira, Erick M.
Angewandte Chemie - International Edition, 2006 , vol. 45, # 46 p. 7736 - 7739
反应条件
1.1: n-BuLi / tetrahydrofuran; hexane / 0.67 h / 0 °C
1.2: tetrahydrofuran; hexane / 60 °C
2.1: 5.15 g / H2 / Rh/C / methanol / 19 h
3.1: n-BuLi / tetrahydrofuran; hexane; diethyl ether / 0.75 h / -78 °C
3.2: triisopropyl borate / tetrahydrofuran; diethyl ether; hexane / -78 - 20 °C
3.3: aq. HCl / tetrahydrofuran; diethyl ether; hexane / 0.33 h
4.1: 83 percent / KOH / [Rh(cod)Cl]2 / dioxane; H2O / 6 h / 20 °C
View Scheme
参考文献
Wuitschik, Georg; Rogers-Evans, Mark; Mueller, Klaus; Fischer, Holger; Wagner, Bjoern; Schuler, Franz; Polonchuk, Liudmila; Carreira, Erick M.
Angewandte Chemie - International Edition, 2006 , vol. 45, # 46 p. 7736 - 7739
