ASP 3026; N2-[2-甲氧基-4-[4-(4-甲基-1-哌嗪基)-1-哌啶基]苯基]-N4-[2-[(1-甲基乙基)磺酰基]苯基]-1,3,5-三嗪-2,4-二胺合成路线 （共 9 条）
反应条件
palladium 10 on activated carbon; hydrogen in tetrahydrofuran T=40°C; P=1861.76 Torr; 7 h; ConcentrationReagent/catalystSolventTemperatureTime;
参考文献
Astellas Pharma Inc.; OBITSU, Kazuyoshi; AKIBA, Takahiro; KOBAYASHI, Koji; HIRASAWA, Shun; KONDOH, Yutaka; TAKEGUCHI, Kazuhiro; TAKAHAMA, Yuji; ORII, Ryoki
Patent: EP2669281 A1, 2013 ;
Location in patent: Paragraph 0059 ;
反应条件
1: 2-methoxy-4-[4-(4-methylpiperazin-1-yl)-piperidin-1-yl]-phenylamine With methanesulfonic acid in ethanol T=20°C; 0.25 h; 2: 1-[1-(3-methoxy-4-nitrophenyl)piperidin-4-yl]-4-methylpiperazine in ethanol T=100°C; 5 h;
参考文献
Astellas Pharma Inc.; OBITSU, Kazuyoshi; AKIBA, Takahiro; KOBAYASHI, Koji; HIRASAWA, Shun; KONDOH, Yutaka; TAKEGUCHI, Kazuhiro; TAKAHAMA, Yuji; ORII, Ryoki
Patent: EP2669281 A1, 2013 ;
Location in patent: Paragraph 0046 ;
反应条件
1: 1,8-diazabicyclo[5.4.0]undec-7-ene / N,N-dimethyl-formamide / 5 h / 20 °C 2: 5 palladium on charcoal; hydrogen / tetrahydrofuran / 3 h / 20 °C / 1500.15 - 2250.23 Torr / |Large scale 3: N-ethyl-N,N-diisopropylamine / tetrahydrofuran / 4 h / 20 °C / |Large scale 4: N-ethyl-N,N-diisopropylamine; hydrogen; palladium 10 on activated carbon / tetrahydrofuran; isopropyl alcohol / 5.5 h / 40 °C / 1861.76 Torr 5: hydrogenchloride; water / tetrahydrofuran; isopropyl alcohol / 17.5 h / 20 °C 6: hydrogen; palladium 10 on activated carbon / tetrahydrofuran / 7 h / 40 °C / 1861.76 Torr View Scheme
反应条件
1.1: 1,2-dichloro-ethane / 0.5 h 1.2: 20 °C 2.1: methanesulfonic acid / ethanol / 0.25 h / 20 °C 2.2: 5 h / 100 °C View Scheme
反应条件
1.1: 5 palladium on charcoal; hydrogen / ethanol / 8 h / 20 °C 2.1: methanesulfonic acid / ethanol / 0.25 h / 20 °C 2.2: 5 h / 100 °C View Scheme
反应条件
1: sodium hydrogencarbonate / acetone / 25 h / 20 °C 2: N-ethyl-N,N-diisopropylamine / tetrahydrofuran / 4 h / 20 °C / |Large scale 3: N-ethyl-N,N-diisopropylamine; hydrogen; palladium 10 on activated carbon / tetrahydrofuran; isopropyl alcohol / 5.5 h / 40 °C / 1861.76 Torr 4: hydrogenchloride; water / tetrahydrofuran; isopropyl alcohol / 17.5 h / 20 °C 5: hydrogen; palladium 10 on activated carbon / tetrahydrofuran / 7 h / 40 °C / 1861.76 Torr View Scheme
反应条件
1: 1,8-diazabicyclo[5.4.0]undec-7-ene / N,N-dimethyl-formamide / 5 h / 20 °C 2: 5 palladium on charcoal; hydrogen / tetrahydrofuran / 3 h / 20 °C / 1500.15 - 2250.23 Torr / |Large scale 3: N-ethyl-N,N-diisopropylamine / tetrahydrofuran / 4 h / 20 °C / |Large scale 4: N-ethyl-N,N-diisopropylamine; hydrogen; palladium 10 on activated carbon / tetrahydrofuran; isopropyl alcohol / 5.5 h / 40 °C / 1861.76 Torr 5: hydrogenchloride; water / tetrahydrofuran; isopropyl alcohol / 17.5 h / 20 °C 6: hydrogen; palladium 10 on activated carbon / tetrahydrofuran / 7 h / 40 °C / 1861.76 Torr View Scheme
反应条件
1: N-ethyl-N,N-diisopropylamine / tetrahydrofuran / 4 h / 20 °C / |Large scale 2: N-ethyl-N,N-diisopropylamine; hydrogen; palladium 10 on activated carbon / tetrahydrofuran; isopropyl alcohol / 5.5 h / 40 °C / 1861.76 Torr 3: hydrogenchloride; water / tetrahydrofuran; isopropyl alcohol / 17.5 h / 20 °C 4: hydrogen; palladium 10 on activated carbon / tetrahydrofuran / 7 h / 40 °C / 1861.76 Torr View Scheme
反应条件
1.1: potassium carbonate / N,N-dimethyl-formamide / 70 °C 2.1: 1,2-dichloro-ethane / 0.5 h 2.2: 20 °C 3.1: 5 palladium on charcoal; hydrogen / ethanol / 8 h / 20 °C 4.1: methanesulfonic acid / ethanol / 0.25 h / 20 °C 4.2: 5 h / 100 °C View Scheme
