二(三甲基甲硅烷基)乙炔合成路线 (共 218 条)
反应条件
pyridine; methyllithium; bromine; lithium bromide 1.) THF, ether, 0 deg C, 30 min; 25 deg C, 30 min, 2.) CH2Cl2, -78 deg C, 15 min; Yield given. Multistep reaction;
参考文献
Mueller, Torsten; Hulliger, Juerg; Seichter, Wilhelm; Weber, Edwin; Weber, Thomas; Wuebbenhorst, Michael
Chemistry - A European Journal, 2000 , vol. 6, # 1 p. 54 - 61
反应条件
1: With methyllithium in diethyl ether T=0 - 20°C; 2: With bromine in diethyl ether; dichloromethane T=-70°C; 0.75 h;
参考文献
Fox, Mark A.; Cameron, Audrey M.; Low, Paul J.; Paterson, Michael A.J.; Batsanov, Andrei S.; Goeta, Andres E.; Rankin, David W.H.; Robertson, Heather E.; Schirlin, Julien T.
Dalton Transactions, 2006 , # 29 p. 3544 - 3560
反应条件
1: carbon monoxide; tri-phenyl-antimony With [bis(acetoxy)iodo]benzene in dichloromethane T=20°C; 7 h; 2: bis(trimethylsilyl)-acetylene With tris(dibenzylideneacetone)dipalladium(0) chloroform complex; copper(l) iodide in acetonitrile T=50°C; 5 h; Further stages.;
参考文献
Kang, Suk-Ku; Ryu, Hyung-Chul; Hong, Young-Taek
Journal of the Chemical Society. Perkin Transactions 1, 2001 , # 7 p. 736 - 739
反应条件
in benzene Irradiation (UV/VIS); (Ar), Schlenk technique, glovebox; soln. irradiated with Hg/Xe arc lamp (400-550 W) for 0.5 h at room temp.; volatiles removed (vac.), residue extd. (hexane), soln. filtered, storedovernight at -30 °C, decanted, filtered (silica gel), volatiles removed (vac.); elem. anal.;
参考文献
Braunschweig, Holger; Fernandez, Israel; Frenking, Gernot; Radacki, Krzysztof; Seeler, Fabian
Angewandte Chemie - International Edition, 2007 , vol. 46, # 27 p. 5215 - 5218
反应条件
in tetrahydrofuran -18°C (40 h), filtering, evapn. (vac.); extg. (hexane), MgCl2 pptn. (-5°C, overnight), concg., crystn. (-18°C, overnight); elem. anal.;
参考文献
Horacek, Michal; Kupfer, Volkmar; Thewalt, Ulf; Stepnicka, Petr; Polasek, Miroslav; Mach, Karel
Organometallics, 1999 , vol. 18, # 18 p. 3572 - 3578
反应条件
copper(l) iodide; tetrakis(triphenylphosphine) palladium(0); tetrabutyl ammonium fluoride; triethylamine in N,N-dimethyl-formamide T=70°C; 8 h; Inert atmosphere;
参考文献
Schmidt, Bernd; Berger, Rene; Kelling, Alexandra; Schilde, Uwe
Chemistry - A European Journal, 2011 , vol. 17, # 25 p. 7032 - 7040
反应条件
aluminium trichloride in neat (no solvent) byproducts: (CH3)3SiCl; allowing a mixture of educts and AlCl3 to stand overnight (thick-walled ampoule, inserted into a steel pipe), heating at 100°C for 6h (vac.), pyrolysis at 800-1200°C (vac. or Ar); EEL-spectroscopy, X-ray diffraction;
参考文献
Maya, Leon; Angelini, Peter
Journal of the American Ceramic Society, 1990 , vol. 73, p. 297 - 302
反应条件
aluminium trichloride in neat (no solvent) byproducts: (CH3)3SiCl, (CH3)3SiCCH; allowing mixture of educts and AlCl3 to stand overnight (thick-walled ampoule, inserted into a steel pipe), heating at 100°C for 6h (vac.), pyrolysis at 800-1200°C (vac. or Ar); EEL-spectroscopy, X-ray diffraction;
参考文献
Maya, Leon; Angelini, Peter
Journal of the American Ceramic Society, 1990 , vol. 73, p. 297 - 302
反应条件
tetrabutylammomium bromide; palladium dichloride in 1-methyl-pyrrolidin-2-one T=100°C; 7 h; Title compound not separated from byproducts;
参考文献
Gil-Molto, Juan; Najera, Carmen
Advanced Synthesis and Catalysis, 2006 , vol. 348, # 14 p. 1874 - 1882
反应条件
1: 1.) CH3Li, LiBr, 2.) Br2, pyridine / 1.) THF, ether, 0 deg C, 30 min; 25 deg C, 30 min, 2.) CH2Cl2, -78 deg C, 15 min 2: 1 percent / pyridine / 25 °C View Scheme
参考文献
Miller, Joseph A.; Zweifel, George
Synthesis, 1983 , # 2 p. 128 - 130