1-溴-2,4,6-三氟苯合成路线 （共 14 条）
反应条件
1: 99 percent / HNO3; H2SO4 / 2 h / 0 °C
2: aq. NH4Cl; Fe / ethanol; tetrahydrofuran / 2 h / Heating
View Scheme
参考文献
Jiang, Yu; Chen, Chien-An; Lu, Kai; Daniewska, Irena; De Leon, John; Kong, Ron; Forray, Carlos; Li, Boshan; Hegde, Laxminarayan G.; Wolinsky, Toni D.; Craig, Douglas A.; Wetzel, John M.; Andersen, Kim; Marzabadi, Mohammad R.
Journal of Medicinal Chemistry, 2007 , vol. 50, # 16 p. 3870 - 3882
反应条件
in tetrahydrofuran
byproducts: MgBrCl; N2 atm.; equimolar ratio, stirring (20°C, overnight); filtn., evapn., washing (n-hexane), dissoln. (CH3CN), addn. of HgCl2, stirring (20°C), sublimation (vac., 65°C); elem. anal.;
参考文献
Layeghi, Hamid; Tyrra, Wieland; Naumann, Dieter
Zeitschrift fur Anorganische und Allgemeine Chemie, 1998 , vol. 624, # 10 p. 1601 - 1610
反应条件
1: 1-bromo-2,4,6-trifluoro-benzene With isopropylmagnesium chloride in tetrahydrofuran
T=20 - 54°C;
2: diethyl 2-oxo-1,3-propanedioate in tetrahydrofuran
T=-55°C; 0.666667 h;
参考文献
BASF Aktiengesellschaft
Patent: US2009/131708 A1, 2009 ;
Location in patent: Page/Page column 2-3 ;
反应条件
1: With magnesium in tetrahydrofuran
T=60°C; 1 h; Inert atmosphereSealed tubeSchlenk technique;
2: With copper(I) bromide in tetrahydrofuran; 1,4-dioxane
T=25 - 40°C; 2.5 h; Inert atmosphereSealed tubeSchlenk technique;
3: in tetrahydrofuran; 1,4-dioxane; toluene
T=80°C; 64 h; Inert atmosphereSealed tubeSchlenk technique;
参考文献
Hofer, Manuel; Gomez-Bengoa, Enrique; Nevado, Cristina
Organometallics, 2014 , vol. 33, # 6 p. 1328 - 1332
