2-溴-5-氟-3-硝基嘧啶合成路线 （共 10 条）
反应条件
N,N-dimethyl-formamide; phosphorus oxytribromide T=20 - 110°C; 3.08333 h;
参考文献
Ueda, Yasutsugu; Connolly, Timothy P.; Kadow, John F.; Meanwell, Nicholas A.; Wang, Tao; Chen, Chung-Pin H.; Yeung, Kap-Sun; Zhang, Zhongxing; Leahy, David Kenneth; Pack, Shawn K.; Soundararajan, Nachimuthu; Sirard, Pierre; Levesque, Kathia; Thoraval, Dominique
Patent: US2005/209246 A1, 2005 ;
Location in patent: Page/Page column 31; 32 ;
反应条件
1.1: tetrafluoroboric acid; sodium nitrite / ethanol; water / 3 h / 0 °C / |Inert atmosphere 1.2: 4 h / 100 °C / |Inert atmosphere 2.1: hydrogenchloride / toluene / 2 h / |Inert atmosphere; |Sealed tube; |Heating 3.1: sulfuric acid; nitric acid / 1 h / 20 - 80 °C / |Inert atmosphere 4.1: phosphorus oxytribromide / N,N-dimethyl-formamide / 3.08 h / 20 - 110 °C / |Inert atmosphere View Scheme
参考文献
Journal of Medicinal Chemistry, , vol. 56, # 4 p. 1656 - 1669
反应条件
1: hydrogenchloride / toluene / 2 h / |Inert atmosphere; |Sealed tube; |Heating 2: sulfuric acid; nitric acid / 1 h / 20 - 80 °C / |Inert atmosphere 3: phosphorus oxytribromide / N,N-dimethyl-formamide / 3.08 h / 20 - 110 °C / |Inert atmosphere View Scheme
参考文献
Journal of Medicinal Chemistry, , vol. 56, # 4 p. 1656 - 1669
反应条件
1: sulfuric acid; nitric acid / 1 h / 20 - 80 °C / |Inert atmosphere 2: phosphorus oxytribromide / N,N-dimethyl-formamide / 3.08 h / 20 - 110 °C / |Inert atmosphere View Scheme
参考文献
Journal of Medicinal Chemistry, , vol. 56, # 4 p. 1656 - 1669
反应条件
hydrogenchloride; tin(ll) chloride in ethanol T=60°C; 1 h;
参考文献
F. HOFFMANN-LA ROCHE AG; ALIAGAS-MARTIN, Ignacio; CRAWFORD, James John; MATHIEU, Simon; RUDOLPH, Joachim; LEE, Wendy
Patent: WO2013/92940 A1, 2013 ;
Location in patent: Page/Page column 50; 51 ;
反应条件
bis-triphenylphosphine-palladium(II) chloride in 1,4-dioxane T=110°C; 16 h; Inert atmosphere;
参考文献
AMGEN INC.
Patent: US2011/152296 A1, 2011 ;
Location in patent: Page/Page column 23 ;
反应条件
1: bis-triphenylphosphine-palladium(II) chloride / 1,4-dioxane / 16 h / 110 °C / Inert atmosphere 2: osmium(VIII) oxide; water; 4-methylmorpholine N-oxide / tert-butyl alcohol; tetrahydrofuran / 6 h / 25 °C 3: sodium periodate; water / tert-butyl alcohol; tetrahydrofuran / 8 h / 25 °C View Scheme
参考文献
AMGEN INC.
Patent: US2011/152296 A1, 2011 ;
反应条件
1: bis-triphenylphosphine-palladium(II) chloride / 1,4-dioxane / 16 h / 110 °C / Inert atmosphere 2: osmium(VIII) oxide; water; 4-methylmorpholine N-oxide / tert-butyl alcohol; tetrahydrofuran / 6 h / 25 °C 3: sodium periodate; water / tert-butyl alcohol; tetrahydrofuran / 8 h / 25 °C 4: toluene-4-sulfonic acid / toluene / 25 - 120 °C 5: hydrogen / palladium on carbon / ethanol / 25 °C / Inert atmosphere 6: water; lithium chloride / dimethyl sulfoxide / 16 h / 90 °C View Scheme
参考文献
AMGEN INC.
Patent: US2011/152296 A1, 2011 ;
反应条件
1: tin(ll) chloride; hydrogenchloride / ethanol / 1 h / 60 °C 2: triethylamine; bis-triphenylphosphine-palladium(II) chloride; copper(l) iodide / tetrahydrofuran / 2 h / 0 - 20 °C / |Inert atmosphere 3: sodium hydride / N,N-dimethyl-formamide; mineral oil / 2 h / 0 - 20 °C / |Inert atmosphere View Scheme
参考文献
F. HOFFMANN-LA ROCHE AG; ALIAGAS-MARTIN, Ignacio; CRAWFORD, James John; MATHIEU, Simon; RUDOLPH, Joachim; LEE, Wendy
Patent: WO2013/92940 A1, 2013 ;
反应条件
in tetrahydrofuran
T=-60 - -40°C; 2.25 h;
参考文献
Ueda, Yasutsugu; Connolly, Timothy P.; Kadow, John F.; Meanwell, Nicholas A.; Wang, Tao; Chen, Chung-Pin H.; Yeung, Kap-Sun; Zhang, Zhongxing; Leahy, David Kenneth; Pack, Shawn K.; Soundararajan, Nachimuthu; Sirard, Pierre; Levesque, Kathia; Thoraval, Dominique
Patent: US2005/209246 A1, 2005 ;
Location in patent: Page/Page column 32 ;
