一水合二对甲苯磺酸拉帕替尼合成路线 （共 28 条）
反应条件
1.1: trichlorophosphate / toluene / 0.17 h / 20 °C / Inert atmosphere 1.2: 3 h / 30 - 75 °C 2.1: isopropyl alcohol / 4 h / 70 °C / Inert atmosphere 3.1: sodium hydroxide / ethyl acetate; water / pH ~ 10 / Inert atmosphere 3.2: 1 h / 40 °C View Scheme
反应条件
1.1: n-butyllithium / ethylene glycol dimethyl ether / 2.75 h / -40 - -35 °C / Inert atmosphere 1.2: 2.5 h / -40 - -35 °C 2.1: N-ethyl-N,N-diisopropylamine; acetic acid / tetrahydrofuran / 2 h / 30 - 35 °C 2.2: 3 h / 20 - 25 °C 3.1: isopropanol acetate / 1 h / 65 - 70 °C View Scheme
反应条件
1.1: acetonitrile / 1 h / |Reflux 2.1: triethylamine; palladium 10 on activated carbon / water; ethylene glycol dimethyl ether; methanol / 45 - 50 °C 3.1: water / 20 - 30 °C 4.1: N-ethyl-N,N-diisopropylamine / methanol / 20 h / 20 - 25 °C 5.1: sodium hydroxide / methanol / 20 h / 20 - 25 °C 6.1: sodium tris(acetoxy)borohydride / tetrahydrofuran / 1 h / 20 - 25 °C 6.3: 3 h View Scheme
反应条件
1.1: acetonitrile / 1 h / |Reflux 2.1: triethylamine; palladium 10 on activated carbon / water; ethylene glycol dimethyl ether; methanol / 45 - 50 °C 3.1: water / 20 - 30 °C 4.1: N-ethyl-N,N-diisopropylamine / methanol / 20 h / 20 - 25 °C 5.1: sodium hydroxide / methanol / 20 h / 20 - 25 °C 6.1: sodium tris(acetoxy)borohydride / tetrahydrofuran / 1 h / 20 - 25 °C 6.3: 3 h View Scheme
反应条件
1.1: triethylamine; palladium 10 on activated carbon / water; ethylene glycol dimethyl ether; methanol / 45 - 50 °C 2.1: water / 20 - 30 °C 3.1: N-ethyl-N,N-diisopropylamine / methanol / 20 h / 20 - 25 °C 4.1: sodium hydroxide / methanol / 20 h / 20 - 25 °C 5.1: sodium tris(acetoxy)borohydride / tetrahydrofuran / 1 h / 20 - 25 °C 5.3: 3 h View Scheme
反应条件
1.1: water / 20 - 30 °C 2.1: N-ethyl-N,N-diisopropylamine / methanol / 20 h / 20 - 25 °C 3.1: sodium hydroxide / methanol / 20 h / 20 - 25 °C 4.1: sodium tris(acetoxy)borohydride / tetrahydrofuran / 1 h / 20 - 25 °C 4.3: 3 h View Scheme
反应条件
1.1: N-ethyl-N,N-diisopropylamine / methanol / 20 h / 20 - 25 °C 2.1: sodium hydroxide / methanol / 20 h / 20 - 25 °C 3.1: sodium tris(acetoxy)borohydride / tetrahydrofuran / 1 h / 20 - 25 °C 3.3: 3 h View Scheme
反应条件
sodium carbonate in water; acetonitrile T=5 - 40°C; 3.58333 h;
参考文献
METSGER, Leonid; MITTELMAN, Ariel; YURKOVSKI, Slavik
Patent: US2010/87459 A1, 2010 ;
Location in patent: Page/Page column 7 ;
