3,3-二氟环丁烷羧酸乙酯合成路线 （共 7 条）
反应条件
1: With lithium aluminium tetrahydride in diethyl ether T=-45 - 20°C; 2: With water; sodium hydroxide in diethyl ether
参考文献
PFIZER LIMITED; GIBSON, Karl Richard; GREEN, Martin Peter; UNDERWOOD, Toby James; WAKENHUT, Florian
Patent: WO2010/32200 A1, 2010 ;
Location in patent: Page/Page column 147-148 ;
WO 2010/032200 A1
反应条件
1: With diisobutylaluminium hydride in hexanes; dichloromethane T=-78°C; 0.75 h; 2: With ammonium chloride in hexanes; dichloromethane; water T=-78 - 20°C;
参考文献
Kazmierski, Wieslaw M.; Maynard, Andrew; Duan, Maosheng; Baskaran, Sam; Botyanszki, Janos; Crosby, Renae; Dickerson, Scott; Tallant, Matthew; Grimes, Rick; Hamatake, Robert; Leivers, Martin; Roberts, Christopher D.; Walker, Jill
Journal of Medicinal Chemistry, 2014 , vol. 57, # 5 p. 2058 - 2073
反应条件
diethylamino-sulfur trifluoride in dichloromethane
T=-4 - 20°C;
参考文献
PFIZER LIMITED; GIBSON, Karl Richard; GREEN, Martin Peter; UNDERWOOD, Toby James; WAKENHUT, Florian
Patent: WO2010/32200 A1, 2010 ;
Location in patent: Page/Page column 147 ;
WO 2010/032200 A1
反应条件
caesium carbonate in N,N-dimethyl-formamide
T=20°C; Inert atmosphere;
参考文献
ASTRAZENECA AB
Patent: US2012/122843 A1, 2012 ;
Location in patent: Page/Page column 40 ;
反应条件
1.1: sodium periodate / RuCl3 monohydrate / dichloromethane; acetonitrile; water / 5 - 20 °C
2.1: diethylamino-sulfur trifluoride / dichloromethane / 24 h / -10 - 20 °C
3.1: sodium hydroxide; water / pentane; methanol / 75 h / 20 - 60 °C
3.2: pH 1
4.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
View Scheme
参考文献
ASTRAZENECA AB
Patent: US2012/122843 A1, 2012 ;
反应条件
1.1: sodium hydroxide; water / pentane; methanol / 75 h / 20 - 60 °C
1.2: pH 1
2.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
View Scheme
参考文献
ASTRAZENECA AB
Patent: US2012/122843 A1, 2012 ;
反应条件
1.1: diethylamino-sulfur trifluoride / dichloromethane / 24 h / -10 - 20 °C
2.1: sodium hydroxide; water / pentane; methanol / 75 h / 20 - 60 °C
2.2: pH 1
3.1: caesium carbonate / N,N-dimethyl-formamide / 20 °C / Inert atmosphere
View Scheme
参考文献
ASTRAZENECA AB
Patent: US2012/122843 A1, 2012 ;
