3,5-二(三氟甲基)硫代苯甲酰胺合成路线 (共 2 条)
反应条件
1: With NaHS monohydrate in N,N-dimethyl-formamide T=10°C; 0.416667 h; Inert atmosphereLarge scale; 2: With MgCl2*6H2O in N,N-dimethyl-formamide T=10°C; 0.833333 h; Large scale; Reagent/catalystTemperatureTime;
参考文献
KARYOPHARM THERAPEUTICS, INC.; SANDANAYAKA, Vincent, P.; SHACHAM, Sharon; MCCAULEY, Dilara; SHECHTER, Sharon
Patent: WO2013/19548 A1, 2013 ;
Location in patent: Page/Page column 83-84 ;
WO 2013/019548 A1
反应条件
1.1: hydrazine hydrate / N,N-dimethyl-formamide / 2 h / 10 °C / |Inert atmosphere; |Large scale 1.2: 13 h / 0 - 100 °C / |Large scale 2.1: 1,4-diaza-bicyclo[2.2.2]octane / N,N-dimethyl-formamide / 0.5 h 2.2: 1 h 3.1: lithium hydroxide hydrate; water / tetrahydrofuran / 4 h / 20 °C 4.1: 1-propanephosphonic acid cyclic anhydride; N-ethyl-N,N-diisopropylamine / dichloromethane; ethyl acetate / 0.5 h / -40 °C View Scheme
参考文献
KARYOPHARM THERAPEUTICS, INC.; SANDANAYAKA, Vincent, P.; SHACHAM, Sharon; MCCAULEY, Dilara; SHECHTER, Sharon
Patent: WO2013/19548 A1, 2013 ;
WO 2013/019548 A1