4,4-二氟乙酰乙酸乙酯合成路线 (共 32 条)
反应条件
1: With sodium ethanolate in ethyl acetate T=25 - 65°C; 2 h; Industry scale; 2: With hydrogenchloride; water in ethyl acetate T=20°C; pH=6 - 7; Industry scale;
参考文献
ELI LILLY AND COMPANY
Patent: US2012/302608 A1, 2012 ;
Location in patent: Page/Page column 4; 5 ;
反应条件
1: With diisopropylamine in tert-butyl methyl ether T=20 - 57°C; 20 h; Heating / reflux; 2: With hydrogenchloride in tert-butyl methyl ether; water T=20 - 25°C; 20 h;
参考文献
BAYER CROPSCIENCE AKTIENGESELLSCHAFT
Patent: WO2005/3077 A1, 2005 ;
Location in patent: Page 12 ;
反应条件
1: ethyl acetate With sodium ethanolate T=25°C; 2: CHF2COOEt T=10 - 65°C; 3: With sulfuric acid; water T=20 - 25°C; 0.333333 h; Product distribution / selectivity;
参考文献
BASF SE
Patent: WO2009/106619 A1, 2009 ;
Location in patent: Page/Page column 7 ;
反应条件
1: ethyl acetate With sodium hydride in ethanol T=20°C; 1 h; 2: N,N-dimethylamino-1,1,2,2-tetrafluoroethane in ethanol T=30°C; 2 h; Product distribution / selectivity;
参考文献
Bayer CropScience AG
Patent: US2010/121095 A1, 2010 ;
Location in patent: Page/Page column 3 ;
反应条件
1: in methanol T=60°C; 3 h; Heating / reflux; 2: With hydrogenchloride in methanol; water T=0°C;
参考文献
WO2006/5612 A1, ;
Page/Page column 7-8 ;
反应条件
1: With sodium ethanolate in ethanol T=60°C; 6 h; 2: With hydrogenchloride in ethanol; water T=0°C; Product distribution / selectivity;
参考文献
SYNGENTA PARTICIPATIONS AG
Patent: WO2006/5612 A1, 2006 ;
Location in patent: Page/Page column 6-7 ;
反应条件
1: With sodium ethanolate in ethanol 1 h; Heating / reflux; 2: With hydrogenchloride in ethanol; water T=0°C; Product distribution / selectivity;
参考文献
SYNGENTA PARTICIPATIONS AG
Patent: WO2006/5612 A1, 2006 ;
Location in patent: Page/Page column 7 ;
反应条件
1: ethyl acetate With lithium diisopropyl amide in tetrahydrofuran T=-78°C; 1 h; 2: methyl 2,2-difluoro-acetate in tetrahydrofuran T=-78°C; 3 h;
参考文献
Jagodzinska, Monika; Huguenot, Florent; Zanda, Matteo
Tetrahedron, 2007 , vol. 63, # 9 p. 2042 - 2046
反应条件
in 1,2-dichloro-ethane T=-15°C;
参考文献
WO2012/7142 A1, ;
Page/Page column 12-13 ;
反应条件
1,1-dibromo ethane; zinc in diethyl ether 1 h; Heating;
参考文献
Dolence; Poulter
Tetrahedron, 1996 , vol. 52, # 1 p. 119 - 130