2-[N,正双(三氟甲烷烷磺酰)氨基]-5-氯吡啶合成路线 （共 16 条）
反应条件
1: NaCH(CO2Et)COCH3 With potassium hexamethylsilazane in N,N-dimethyl-formamide T=0°C; 0.0833333 h; 2: N-(5-chloropyridin-2-yl)-1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide in N,N-dimethyl-formamide T=0 - 20°C; 12 h;
参考文献
PURDUE RESEARCH FOUNDATION
Patent: WO2006/99313 A2, 2006 ;
Location in patent: Page/Page column 32 ;
WO 2006/099313 A2
反应条件
1: (tert-Butoxycarbonyl)piperidin-3-one With n-butyllithium; diisopropylamine in tetrahydrofuran; hexane
T=-78°C; 0.5 h; Inert atmosphere;
2: N-(5-chloropyridin-2-yl)-1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide in tetrahydrofuran; hexane
T=-78 - 20°C; Inert atmosphere;
参考文献
JANSSEN RandD IRELAND; GUILLEMONT, Jerôme Emile Georges; LANÇOIS, David Francis Alain; MOTTE, Magali Madeleine Simone; BALEMANS, Wendy Mia Albert; KOUL, Anil
Patent: WO2014/23815 A1, 2014 ;
Location in patent: Page/Page column 42; 43 ;
反应条件
lithium diisopropyl amide
1.) THF 2.) -78 deg C, 2 h or -23 deg C, 4 h or -16 deg C, 12 h; Yield given. Multistep reaction;
参考文献
Comins, Daniel L.; Dehghani, Ali
Tetrahedron Letters, 1992 , vol. 33, # 42 p. 6299 - 6302
反应条件
1: 4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexanone With lithium diisopropyl amide in tetrahydrofuran
T=-78°C; 0.5 h;
2: N-(5-chloropyridin-2-yl)-1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide in tetrahydrofuran
T=-78°C; 2 h;
参考文献
SANOFI; GAO, Zhongli
Patent: WO2011/143150 A1, 2011 ;
Location in patent: Page/Page column 46-47 ;
WO 2011/143150 A1
反应条件
lithium hexamethyldisilazane in tetrahydrofuran
T=-78 - -20°C;
参考文献
Honda, Toshio; Takahashi, Rie; Namiki, Hidenori
Journal of Organic Chemistry, 2005 , vol. 70, # 2 p. 499 - 504
反应条件
1: 3-Oxo-pyrrolidine-1-carboxylic acid tert-butyl ester With lithium hexamethyldisilazane in tetrahydrofuran
T=-78°C; 1 h;
2: N-(5-chloropyridin-2-yl)-1,1,1-trifluoro-N-[(trifluoromethyl)sulfonyl]methanesulfonamide in tetrahydrofuran
T=-78 - 20°C; 3.5 h;
参考文献
Purandare, Ashok Vinayak; Wan, Honghe; Huynh, Tram N.
Patent: US2006/235037 A1, 2006 ;
Location in patent: Page/Page column 60 ;
US 20060235037 A1
