triethylamine in benzene
byproducts: Et3N*HCl; dropwise addn. of mixt. of Si-compd. and Et3N to GeCl4 soln., stirring (24 h, 20°C), heating to 80°C for 30 min (Et3N*HCl removal); distn.; elem. anal.;
参考文献
Riviere-Baudet, Monique; Khallaayoun, Abdelhay; Ahra, Mohamed
Phosphorus, Sulfur and Silicon and the Related Elements, 1993 , vol. 81, # 1-4 p. 95 - 100
magnesium in tetrahydrofuran
byproducts: MgCl2; (1) vinyl chloride bubbled through a suspn. of Mg in an inert atmosphere, the react. initiated with 1,2-dibromoethane and performed at 55-60°C (25-30°C by the end); (2) a soln. of GeCl4 added dropwise at temp. not exceeding 30°C; kept at 20-30°C for 6 h; treated with H2O, the aq. layer sepd., the org. layer washed (H2O), distd. fractionally to give mixts.;
参考文献
Zhun'; Sbitneva; Kisin; Chernyshev
Russian Journal of General Chemistry, 2004 , vol. 74, # 7 p. 1130 - 1131
magnesium in tetrahydrofuran
byproducts: MgCl2; (1) vinyl chloride bubbled through a suspn. of Mg in an inert atmosphere, the react. initiated with 1,2-dibromoethane and performed at 55-60°C (25-30°C by the end); (2) a soln. of GeCl4 added dropwise at temp. not exceeding 30°C; kept at 20-30°C for 6 h; treated with H2O, the aq. layer sepd., the org. layer washed (H2O), distd. fractionally to give mixts.;
参考文献
Zhun'; Sbitneva; Kisin; Chernyshev
Russian Journal of General Chemistry, 2004 , vol. 74, # 7 p. 1130 - 1131
Chernyshev, E. A.; Komalenkova, N. G.; Yakovleva, G. N.
Doklady Chemistry (English Translation), 1994 , vol. 336, p. 88 - 89
Doklady Akademii Nauk SSSR, 1994 , vol. 336, p. 69 - 70
2,2'-azobisisobutyronitrile in neat (no solvent)
standard Schlenk technique; flask with 2,2'-azobisisobutyronitrile and CH2CHSnBu3 was cooled to -78°C and evacuated; GeCl4 was added; mixt. was heated at 90°C for 3 h; distd. (vac.);
参考文献
Faller; Kultyshev, Roman G.
Organometallics, 2002 , vol. 21, # 26 p. 5911 - 5918
(E)-vinyl chloride in neat (no solvent)
600-700°C, in presence of HSiCl3;
参考文献
Shcherbinin, V. V.; Shvedov, I. P.; Pavlov, K. V.; Mironov, V. F.
Russian Journal of General Chemistry, 1993 , vol. 63, p. 1336 - 1336
Zhurnal Obshchei Khimii, 1993 , vol. 63, p. 1915 - 1916
n-butyllithium in tetrahydrofuran; benzene
equimolar amt. of BuLi added to a soln. of furan in THF at 0°C; soln. immediately turned yellow; resulting mixt. stirred for 30 min at 0°C; soln. of GeCl4 in C6H6 added at 0°C and mixt. stirred for another 3 h at 25°C; mixt. poured into H2O and extd. with EtOAc; combined org. layer dried and concd. in vacuo; recrystn. from toluene;
参考文献
Nakamura; Yorimitsu; Shinokubo; Oshima
Bulletin of the Chemical Society of Japan, 2001 , vol. 74, # 4 p. 747 - 752
in tetrahydrofuran; hexane; benzene
under Ar; n-BuLi/hexane added to soln. of furan in THF at 0°C, mixt. stirred at 0°C for 30 min, soln. of GeCl4 in benzene slowly added at 0°C, mixt. stirred at 25°C for 3 h; mixt. poured into water, extn. with EtOAc, combined org. phases dried, concd. under vac., column chromy. (silica gel); elem. anal.;
water in not given
N2-atmopshere; dropwise addn. MesMgBr to GeCl4, refluxing (overnight), H2O addn.; washing (H2O), drying (MgSO4), evapn., reacrystn. (EtOH);
参考文献
Lambert, Joseph B.; Zhao, Yan; Wu, Hongwei; Tse, Winston C.; Kuhlmann, Barbara
Journal of the American Chemical Society, 1999 , vol. 121, # 21 p. 5001 - 5008
