1,4-二氯-5,6,7,8-四氢-5,8-乙烷酞嗪合成路线 （共 6 条）
反应条件
trichlorophosphate T=110°C; 5 h;
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; XIE, Hongming; REN, Qingyun; TAN, Yumei; LUO, Huichao
Patent: WO2014/19344 A1, 2014 ;
Location in patent: Paragraph 00417 ;
反应条件
1.1: tetrahydrofuran / 18 h / 60 °C 2.1: palladium on activated charcoal; hydrogen / ethyl acetate / 2 h 3.1: sodium hydroxide; water / methanol / 8 h / 60 °C 3.2: pH 1 4.1: acetic anhydride / 1.5 h / 100 °C 5.1: hydrazine hydrate; acetic acid; sodium acetate / 16 h / 100 °C 6.1: trichlorophosphate / 5 h / 110 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; XIE, Hongming; REN, Qingyun; TAN, Yumei; LUO, Huichao
Patent: WO2014/19344 A1, 2014 ;
反应条件
1.1: palladium on activated charcoal; hydrogen / ethyl acetate / 2 h 2.1: sodium hydroxide; water / methanol / 8 h / 60 °C 2.2: pH 1 3.1: acetic anhydride / 1.5 h / 100 °C 4.1: hydrazine hydrate; acetic acid; sodium acetate / 16 h / 100 °C 5.1: trichlorophosphate / 5 h / 110 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; XIE, Hongming; REN, Qingyun; TAN, Yumei; LUO, Huichao
Patent: WO2014/19344 A1, 2014 ;
反应条件
1.1: sodium hydroxide; water / methanol / 8 h / 60 °C 1.2: pH 1 2.1: acetic anhydride / 1.5 h / 100 °C 3.1: hydrazine hydrate; acetic acid; sodium acetate / 16 h / 100 °C 4.1: trichlorophosphate / 5 h / 110 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; XIE, Hongming; REN, Qingyun; TAN, Yumei; LUO, Huichao
Patent: WO2014/19344 A1, 2014 ;
反应条件
1: hydrazine hydrate; acetic acid; sodium acetate / 16 h / 100 °C 2: trichlorophosphate / 5 h / 110 °C View Scheme
参考文献
SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; XIE, Hongming; REN, Qingyun; TAN, Yumei; LUO, Huichao
Patent: WO2014/19344 A1, 2014 ;
反应条件
hydrazine hydrate in ethanol
18 h; Heating;
参考文献
Russell, Michael G. N.; Carling, Robert W.; Atack, John R.; Bromidge, Frances A.; Cook, Susan M.; Hunt, Peter; Isted, Catherine; Lucas, Matt; McKernan, Ruth M.; Mitchinson, Andrew; Moore, Kevin W.; Narquizian, Robert; Macaulay, Alison J.; Thomas, David; Thompson, Sally-Anne; Wafford, Keith A.; Castro, Jose L.
Journal of Medicinal Chemistry, 2005 , vol. 48, # 5 p. 1367 - 1383
