in tetrahydrofuran LiSnMe3 added to PhGeMe3 in THF, stirred at 24°C for 1 h or 50°C for 30 min, hydrolysis with water; org. layer extd. with ether, dried over Na2SO4; products isolated by preparative by GLC;
参考文献
Bulletin of the Chemical Society of Japan, , vol. 60, # 9 p. 3299 - 3306
in tetrahydrofuran LiSnMe3 added to PhGeMe3 in THF, stirred at 24°C for 1 h or 50°C for 30 min, hydrolysis with water; org. layer extd. with ether, dried over Na2SO4; products isolated by preparative by GLC;
参考文献
Bulletin of the Chemical Society of Japan, , vol. 60, # 9 p. 3299 - 3306
in tetrahydrofuran LiSnMe3 added to PhGeMe3 in THF, stirred at 24°C for 1 h or 50°C for 30 min, hydrolysis with water; org. layer extd. with ether, dried over Na2SO4; products isolated by preparative by GLC;
参考文献
Mochida, Kunio
Bulletin of the Chemical Society of Japan, 1987 , vol. 60, # 9 p. 3299 - 3306
magnesium in tetrahydrofuran
byproducts: MgBr2; Sonication; the mixt. of magnesium, germane and halogen-compound in THF was sonicated for 2 h (inert atm.); the mixt. was washed with satd. soln. of NaCl, extd. with diethyl ether,the organic layer was dried over MgSO4, the solvent was removed under r educed pressure, column chromy. (petroleum ether-diethyl ether 95/5);
magnesium; methyl iodide in tetrahydrofuran
THF soln. of PhBr was added dropwise to Mg metal, reaction was initiated with MeI, stirred for 2 h at 25°C under Ar, a soln. of Me3GeCl in THF was added dropwise, mixt. was refluxed for 2 h; cooled, treated with 5percent aq. NH4Cl, extd. with CH2Cl2, ext. was washed with water, dried (Na2SO4), fractionated; elem. anal.;
参考文献
Moerlein, S. M.
Journal of Organometallic Chemistry, 1987 , vol. 319, p. 29 - 40
Mg in tetrahydrofuran
under high-vac. techniques; mixt. of bromobenzene, C6H5CH2SnMe3 and Mg in THF stirred for 26 h at room temp.; quenched with Me3GeCl; Et2O added; org. and aq. fractions sepd.; org. fraction dried (MgSO4); analyzed by NMR; sepd. by chromy.;
参考文献
Van Klink, Gerard P.M.; De Boer, Henricus J.R.; Schat, Gerrit; Akkerman, Otto S.; Bickelhaupt, Friedrich; Spek, Anthony L.
Organometallics, 2002 , vol. 21, # 10 p. 2119 - 2135
tetrachloromethane in cyclohexane
Irradiation (UV/VIS); irradiation of catenate in cyclohexane containing CCl4 with a 110 W low-pressure Hg arc lamp at room temp. under Ar for 1-4 h; identification by GC and GC-MS;
参考文献
Mochida, Kunio; Kikkawa, Haruhiko; Nakadaira, Yasuhiro
Journal of Organometallic Chemistry, 1991 , vol. 412, # 1.2 p. 9 - 19
in cyclohexane
Irradiation (UV/VIS); irradiation of catenate in cyclohexane with a 110 W low-pressure Hg arc lamp at room temp. under Ar for 1-4 h, further products; identification by GC and GC-MS;
参考文献
Mochida, Kunio; Kikkawa, Haruhiko; Nakadaira, Yasuhiro
Journal of Organometallic Chemistry, 1991 , vol. 412, # 1.2 p. 9 - 19
→
反应条件
in pentane
C6H5Li, pentane, Ar; preparative GC/MS;
参考文献
Zharov, Ilya; Weng, Tsu-Chien; Orendt, Anita M.; Barich, Dewey H.; Penner-Hahn, James; Grant, David M.; Havlas, Zdenek; Michl, Josef
Journal of the American Chemical Society, 2004 , vol. 126, # 38 p. 12033 - 12046
bromobenzene; water; calcium in gas
Ca vaporized at 900°C in vac. (ca. 5E-3 Torr), Me3GeGeMe3 introduced as vapor, mixed vapors condensed on cold (77 K) walls, warmed to room temp., excess of C6H5Br admitted as vapor, left to stand for 1 h, hydrolyzed with water; org layer extd. with ether, products identified by GC-MASS, GLC;
参考文献
Mochida, Kunio; Yamanishi, Takayuki
Bulletin of the Chemical Society of Japan, 1987 , vol. 60, # 9 p. 3429 - 3430
