反应条件
Mg in tetrahydrofuran byproducts: MgBr2; under dry N2 or Ar; PhMgBr-Grignard in THF (Mg excess separated), addn.of GeCl4 in THF (2 h), stirred (refluxed, 12 h), addn. of H2O and 2 N HCl,sepn. of organic layers, extn. of H2O layer with CHCl3 (three times); evapn. of organic phases, dried (120°C, several h), soln. (CHCl3), chromy. (SiO2, CHCl3), concn., cooled (-40°C), crystn. of GePh4, concn., addn. of ether, sublimation or chromy. (SiO2, heptane/CH2Cl2), fractionated crystn.;
参考文献
Journal of Organometallic Chemistry, , vol. 301, p. 27 - 40
