in diethyl ether under N2 a soln. of a mixt. of Ph3GeCl and Ph2GeCl2 was treated with an excess of LiAlH4; after hydrolysis the organic layer was dried over Na2SO4, pumped off, chromd. (silica gel, benzene/hexane);
参考文献
Cerveau, Genevieve; Colomer, Ernesto; Corriu, Robert J.P.; Young, J. Colin
Journal of Organometallic Chemistry, 1981 , vol. 205, # 1 p. 31 - 45
according to R. L. Dannley, G. C. Farrant, G. C. J. Org. Chem. 34 (1969)2428;
参考文献
Thomas, John Meurig; Sankar, Gopinathan; Klunduk, Marek C.; Attfield, Martin P.; Maschmeyer, Thomas; Johnson, Brian F. G.; Bell, Robert G.
Journal of Physical Chemistry B, 1999 , vol. 103, # 42 p. 8809 - 8813
in ethylene glycol dimethyl ether Electrolysis; (N2); potential controlled electrolysis at -2,0 V (vs. AgI/Ag referenceelectrode) of soln. of Ge compd. at room temp.; filtered soln. was evapd. in vac., residue was extd. with ether and solvent removed, residue was sepd. by TLC, products were identified by m. p., IR, NMR and MAS;
参考文献
Journal of Organometallic Chemistry, , vol. 188, # 1 p. 63 - 72
→
反应条件
in diethyl ether; acetonitrile byproducts: H2O; addn. of soln. of Mo-compd. in MeCn to soln. of Ge-compd. in MeCN, addn. of Et2O, standing (2-3 days); evapn., extn. (chloroform), recrystn. of residue (MeCN-Et2O, 0°C); elem. anal.;
参考文献
Bhattacharyya, R. G.; Biswas, S.
Inorganica Chimica Acta, 1991 , vol. 181, p. 213 - 216
in N,N-dimethyl-formamide Sonication; glove box under N2; mixed, ultrasonication at 25+/-5°C; centrifuged, washed (pentane or hexane), extd. (three times with pentane or hexane), evapd., recrystd. (hexane); elem. anal.;
参考文献
Cochran, John C.; Lemieux, Robert P.; Giacobbe, Robert C.; Roitstein, Alexander
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 1990 , vol. 20, p. 251 - 262