2-(甲硫基)-4,6-二氯-5-嘧啶甲醛合成路线 （共 15 条）
反应条件
1: N,N-dimethyl-formamide With trichlorophosphate in 1,1,2-trichloroethylene T=5 - 20°C; 2: 2,4-dihydroxy-2-methylmercaptopyrimidine (zwitterionic form) in 1,1,2-trichloroethylene T=80°C;
参考文献
WO2006/104889 A2, ;
Page/Page column 113-114 ;
WO 2006/104889 A2
反应条件
trichlorophosphate in 1,1,2-trichloroethylene T=5 - 80°C;
参考文献
WO2007/147104 A2, ;
Page/Page column 78-79 ;
WO 2007/147104 A2
反应条件
1: N,N-dimethyl-formamide With trichlorophosphate T=-5 - 20°C; 1 h; 2: 2-methylmercapto-4,6-dihydroxypyrimidine T=20°C; 3.5 h; Heating / reflux;
参考文献
WO2007/84560 A2, ;
Page/Page column 105-106 ;
反应条件
1: N,N-dimethyl-formamide With trichlorophosphate T=0 - 20°C; 0.5 h; 2: 2-mercapto-4,6-dihydroxy-pyrimidine T=20°C; 7 h; Heating / reflux;
参考文献
EP1970373 A1, ;
Page/Page column 35 ;
反应条件
sodium chlorite; aminosulfonic acid in tetrahydrofuran; water; tert-butyl alcohol T=-10 - 35°C; 0.166667 h;
参考文献
Takeda Pharmaceutical Company Limited
Patent: EP2471793 A1, 2012 ;
Location in patent: Page/Page column 58 ;
反应条件
1: aminosulfonic acid; sodium chlorite / water; tert-butyl alcohol; tetrahydrofuran / 0.17 h / -10 - 35 °C 2: oxalyl dichloride / N,N-dimethyl-formamide / toluene / 1 h / 10 - 35 °C 3: triethylamine / 2 h / 10 - 35 °C View Scheme
参考文献
Takeda Pharmaceutical Company Limited
Patent: EP2471793 A1, 2012 ;
反应条件
hydroxylamine hydrochloride; acetic acid in ethanol T=20 - 60°C; 2 h;
参考文献
Wan, Zehong; Yan, Hongxing; Hall, Ralph F.; Lin, Xichen; Livia, Stefano; Respondek, Tomasz; Widdowson, Katherine L.; Zhu, Chongjie; Callahan, James F.
Tetrahedron Letters, 2009 , vol. 50, # 3 p. 370 - 372
反应条件
triethylamine in ethanol T=18 - 25°C; 1 h;
参考文献
ASTRAZENECA AB; ASTRAZENECA UK LIMITED; CHUAQUI, Claudio, Edmundo; HUANG, Shan; IOANNIDIS, Stephanos; SHI, Jie; SU, Mei; SU, Qibin
Patent: WO2010/38060 A1, 2010 ;
Location in patent: Page/Page column 73 ;
WO 2010/038060 A1
反应条件
hydrazine hydrate; triethylamine in 1,4-dioxane
T=20°C; 5 h;
参考文献
Vignaroli, Giulia; Mencarelli, Martina; Sementa, Deborah; Crespan, Emmanuele; Kissova, Miroslava; Maga, Giovanni; Schenone, Silvia; Radi, Marco; Botta, Maurizio
ACS Combinatorial Science, 2014 , vol. 16, # 4 p. 168 - 175
反应条件
sodium hydride in dimethyl sulfoxide
T=23°C; 3 h;
参考文献
Adams, Jerry L.; Boehm, Jeffrey C.; Hall, Ralph; Jin, Qi; Kasparec, Jiri; Silva, Domingos J.; Taggart, John J.
Patent: US2004/116697 A1, 2004 ;
Location in patent: Page 22 ;
US 20040116697 A1
