14-羟基二氢降吗啡酮盐酸盐 合成路线 (共 10 条)
反应条件
triethylamine in 1-methyl-pyrrolidin-2-one; water T=70°C; 9.5 h; Inert atmosphere;
参考文献
US2012/283443 A1, ;
Page/Page column 18 ;
反应条件
sodium hydrogencarbonate; sodium carbonate; sodium bromide in 1-methyl-pyrrolidin-2-one; water T=30°C; 16 h;
参考文献
US2011/269964 A1, ;
Page/Page column 9 ;
反应条件
acetic acid; 1,4-di(diphenylphosphino)-butane; palladium diacetate in N,N-dimethyl-formamide T=50°C; 16 h; Product distribution / selectivity;
参考文献
WO2011/154827 A2, ;
Page/Page column 166 ;
反应条件
1: in acetonitrile T=20°C; 16 h; 2: With formic acid; triethylamine in acetonitrile T=20°C; 24.5 h; Product distribution / selectivity;
参考文献
MALLINCKRODT INC.
Patent: WO2008/137672 A1, 2008 ;
Location in patent: Page/Page column 23 ;
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反应条件
342884-62-2 22-(2-甲基-2-丙烯-1-基)-14-氧杂-11,22-二氮杂七环[13.9.1.01,13.02,21.04,12.05,10.019,25]二十五-4(12),5,7,9,15(25),16,18-七烯-2,16-二醇盐酸盐(1:1)
反应条件
1: 85 percent / NaHCO3 / dimethylformamide / 2 h / 80 °C 2: 97 percent / 3 N HCl / methanol / 12 h / 80 °C View Scheme
参考文献
Ullrich; Dersch; Rothman; Jacobson; Rice
Bioorganic and medicinal chemistry letters, 2001 , vol. 11, # 21 p. 2883 - 2885
反应条件
1: in acetonitrile 0.0833333 h; 2: With formic acid; triethylamine; [Ru2(p-PriC6H4Me)2(μ-Cl)Cl]2 in acetonitrile T=20°C; 3: With ammonia in water pH=9.4; Product distribution / selectivity;
参考文献
Mallinckrodt Inc.
Patent: US2010/81817 A1, 2010 ;
Location in patent: Page/Page column 12 ;
反应条件
N-ethyl-N,N-diisopropylamine in 1-ethyl-2-pyrrolidinone T=52 - 57°C; 24.75 h; Product distribution / selectivity;
参考文献
H. Lundbeck A/S
Patent: US2012/116085 A1, 2012 ;
Location in patent: Page/Page column 6 ;
反应条件
1: cyclopropyl carbinol With methanesulfonyl chloride; triethylamine in N,N-dimethyl-formamide T=0 - 5°C; 3 h; 2: With lithium bromide in N,N-dimethyl-formamide T=0 - 15°C; 3: 14-hydroxydihydronormorphinone in N,N-dimethyl-formamide T=0 - 70°C;
参考文献
SUN PHARMACEUTICAL INDUSTRIES LTD.
Patent: WO2009/122436 A2, 2009 ;
Location in patent: Page/Page column 32-33 ;
反应条件
sodium hydrogencarbonate; N-methyl-tri-n-butyl-ammonium bromide; sodium bromide in isobutyramide; water T=85°C; 2.5 h; Product distribution / selectivity;
参考文献
Mallinckrodt Inc.
Patent: US2011/269964 A1, 2011 ;
Location in patent: Page/Page column 9 ;
反应条件
1: With hydrogen; platinum on activated charcoal in 1-methyl-pyrrolidin-2-one; methanol T=50°C; P=2068.65 Torr; 1 h; 2: With hydrogenchloride in ethanol; water pH=< 4; Product distribution / selectivity;
参考文献
WO2006/35195 A1, ;
Page/Page column 7 ;