外消旋5-羟甲基去异丙基托特罗定-d6合成路线 （共 69 条）
反应条件
hydrogen; 5 Pd(II)/C(eggshell) in methanol T=50 - 55°C;
参考文献
ACTAVIS GROUP PTC EHF
Patent: US2010/217034 A1, 2010 ;
Location in patent: Page/Page column 10 ;
反应条件
1: With sodium hydrogencarbonate in ethyl acetate Inert atmosphere; 2: With lithium aluminium tetrahydride in tetrahydrofuran T=20°C; 3.5 h; 3: With ammonium chloride in tetrahydrofuran T=-10 - 20°C; 0.5 h;
参考文献
DIPHARMA FRANCIS S.r.I.
Patent: US2011/105783 A1, 2011 ;
Location in patent: Page/Page column 6 ;
反应条件
1: With hydrogen; palladium on activated charcoal in methanol T=20°C; P=3000.3 Torr; 18 h; 2: With lithium aluminium tetrahydride in tetrahydrofuran 3: With water in tetrahydrofuran
参考文献
WO2007/144097 A1, ;
Page/Page column 21 ;
反应条件
1: With water; sodium hydroxide in dichloromethane pH=7 - 8; 2: With lithium aluminium tetrahydride in tetrahydrofuran T=0 - 25°C;
参考文献
CRYSTAL PHARMA, S.A.U.; LORENTE BONDE-LARSEN, Antonio; GALLO NIETO, Francisco Javier; FERREIRO GIL, Juan José; MARTÍN PASCUAL, Pablo
Patent: WO2013/113946 A2, 2013 ;
Location in patent: Page/Page column 35 ;
反应条件
potassium carbonate in toluene T=50°C; 2 h;
参考文献
CHEMI S.P.A.; Ciambecchini, Umberto; Turchetta, Stefano; De Ferra, Lorenzo; Zenoni, Maurizio
Patent: US2013/79532 A1, 2013 ;
Location in patent: Paragraph 0081; 0082 ;
反应条件
1: With (+)-(R)-malic acid in di-isopropyl ether; isopropyl alcohol T=20 - 80°C; 2: With sodium hydrogencarbonate in water pH=10; Product distribution / selectivity;
参考文献
PANACEA BIOTEC LTD; JAIN, Rajesh; RAO, SIripragada, Mahender; RAO, Jagadeeshwar, R.; MADADA, Chandra, Rao
Patent: WO2011/158257 A1, 2011 ;
Location in patent: Page/Page column 34 ;
反应条件
water; lithium hydroxide hydrate in methanol T=25 - 35°C; 4 h;
参考文献
WO2012/98560 A2, ;
Page/Page column 69 ;
WO 2012/098560 A2
反应条件
sodium tetrahydroborate in methanol Product distribution / selectivity;
参考文献
LEK PHARMACEUTICALS D.D.
Patent: WO2007/147547 A1, 2007 ;
Location in patent: Page/Page column 15 ;
WO 2007/147547 A1
反应条件
1.1: methanesulfonic acid / 50 - 55 °C / Inert atmosphere 2.1: ethanol / 20 - 60 °C / Inert atmosphere 3.1: sodium hydrogencarbonate / ethyl acetate / Inert atmosphere 3.2: 3.5 h / 20 °C 3.3: 0.5 h / -10 - 20 °C View Scheme
反应条件
1: lithium aluminium tetrahydride / tetrahydrofuran / 14 h / 25 - 30 °C 2: hydrogen / 5 Pd(II)/C(eggshell) / methanol / 50 - 55 °C View Scheme
