in n-heptane byproducts: NaBr; under dry Ar or N2, 3 equiv. of Na-compd. and AlBr3 were mixed in heptane at -78 °C, heating at room temp. for 24 h; soln. was filtered, filtrate was concd., crystn. at -23 °C for a week, elem. anal.;
参考文献
Wiberg, Nils; Blank, Thomas; Amelunxen, Kerstin; Noeth, Heinrich; Schnoeckel, Hansgeorg; et al.
European Journal of Inorganic Chemistry, 2002 , p. 341 - 350
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反应条件
in tetrahydrofuran mixed (-70°C), stirred overnight; salt filtn., filtrate condensing (vac.), crystn. (heptane), chromy. (GPCin toluene); elem. anal.;
参考文献
Sekiguchi, Akira; Yamazaki, Hajime; Kabuto, Chizuko; Sakurai, Hideki; Nagase, Shigeru
Journal of the American Chemical Society, 1995 , vol. 117, # 30 p. 8025 - 8026
1: 90 percent / Br2 / pentane / 0 °C 2: 58 percent / Na / heptane / 3 h / Heating 3: heptane / 12 h / 100 °C / dependence of product distribution on time, temperature, solvents or in absence of tri-terc-butyl silyl-halogenide View Scheme
1: 91 percent / KHF2, KF / 5 h / 70 °C 2: 86 percent / heptane; pentane / 6 h 3: 90 percent / Br2 / pentane / 0 °C 4: 58 percent / Na / heptane / 3 h / Heating 5: heptane / 12 h / 100 °C / dependence of product distribution on time, temperature, solvents or in absence of tri-terc-butyl silyl-halogenide View Scheme
in tetrahydrofuran byproducts: NaBr; under dry Ar or N2, 3 equiv. of Na-compd. and InCl3 were mixed in THF at-78 °C, heating to room temp. over 5 h; THF was changed to toluene, soln. was filtered, filtrate was concd., crystn. at -23 °C for several days, elem. anal.;
参考文献
Wiberg, Nils; Blank, Thomas; Amelunxen, Kerstin; Noeth, Heinrich; Schnoeckel, Hansgeorg; et al.
European Journal of Inorganic Chemistry, 2002 , p. 341 - 350
in n-heptane byproducts: (t-Bu)3SiH; under dry Ar or N2, 90 °C for 7 h; volatiles were removed in vac., residue was taken in heptane, soln. was filtered, concd., crystn. at -23 °C, elem. anal.;
参考文献
Wiberg, Nils; Blank, Thomas; Amelunxen, Kerstin; Noeth, Heinrich; Schnoeckel, Hansgeorg; et al.
European Journal of Inorganic Chemistry, 2002 , p. 341 - 350
in pentane byproducts: NaBr; under dry Ar or N2, -30 °C, warming to room temp. over 24 h; NaCl was filtered off, filtrate was concd., cooled to -23 °C, ((t-Bu3)Si)2 was sepd., crystn. for 5 d;
参考文献
Wiberg, Nils; Blank, Thomas; Amelunxen, Kerstin; Noeth, Heinrich; Schnoeckel, Hansgeorg; et al.
European Journal of Inorganic Chemistry, 2002 , p. 341 - 350
