2-氯-N,3-二甲基-N-苯基-4-吡啶羧酰胺合成路线 (共 5 条)
反应条件
1: With n-butyllithium in tetrahydrofuran; hexane T=-78°C; 0.5 h; 2: With methyl iodide in tetrahydrofuran; hexane T=-78 - 33°C; 1.5 h;
参考文献
ACTELION PHARMACEUTICALS LTD
Patent: WO2005/54244 A2, 2005 ;
Location in patent: Page/Page column 23 ;
反应条件
1: 2-chloro-N-phenylisonicotinamide With n-butyllithium in tetrahydrofuran; hexane T=-70 - -65°C; 2.5 h; 2: methyl iodide in tetrahydrofuran; hexane T=-78 - 33°C; 1.5 h;
参考文献
ACTELION PHARMACEUTICALS LTD.
Patent: WO2006/21402 A1, 2006 ;
Location in patent: Page/Page column 44 ;
WO 2006/021402 A1
反应条件
1: 2-chloro-N-phenylisonicotinamide With n-butyllithium in tetrahydrofuran; hexanes T=-78°C; 1.23333 h; Inert atmosphere; 2: methyl iodide in tetrahydrofuran; hexanes T=-78 - 20°C; 21.1333 h;
参考文献
EPIZYME, INC.; EISAI CO., LTD.; KUNTZ, Kevin, Wayne; CHESWORTH, Richard; DUNCAN, Kenneth, William; KEILHACK, Heike; WARHOLIC, Natalie; KLAUS, Christine; ZHENG, Wanjun
Patent: WO2012/142513 A1, 2012 ;
Location in patent: Page/Page column 427 ;
WO 2012/142513 A1
反应条件
1.1: sulfuric acid / water / 46 h / 130 °C 1.2: pH 8 1.3: pH 3 2.1: potassium carbonate / N,N-dimethyl-formamide / 18.5 h / 20 °C / Inert atmosphere View Scheme
参考文献
EPIZYME, INC.; EISAI CO., LTD.; KUNTZ, Kevin, Wayne; CHESWORTH, Richard; DUNCAN, Kenneth, William; KEILHACK, Heike; WARHOLIC, Natalie; KLAUS, Christine; ZHENG, Wanjun
Patent: WO2012/142513 A1, 2012 ;
WO 2012/142513 A1
反应条件
diisobutylaluminium hydride in tetrahydrofuran; dichloromethane
T=-78 - -60°C; 3.5 h;
参考文献
ACTELION PHARMACEUTICALS LTD
Patent: WO2006/21403 A1, 2006 ;
Location in patent: Page/Page column 20-21 ;
WO 2006/021403 A1