Technology Process of Ph3GeGePh2GePh3
There total 9 articles about Ph3GeGePh2GePh3 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
diethyl ether;
Ph3GeLi (prepd. from Ph3GeH and BuLi) was added to Ph2GeCl2 in ether under Ar, mixt. was heated under reflux (35°C) for 1 h; reaction mixt. was hydrolyzed, extd. with ether. ext. dried over Na2SO4, concd. under reduced pressure, residue was recrystd.;
DOI:10.1016/S0022-328X(00)98750-3
- Guidance literature:
-
With
potassium;
In
tetrahydrofuran; N,N,N,N,N,N-hexamethylphosphoric triamide;
byproducts: KCl; reaction between Ge2Ph6 and K at 20°C for 5 h; addn. of Ph2GeCl2 at -50°C;;
DOI:10.1016/S0022-328X(00)99705-5
- Guidance literature:
-
With
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.;
DOI:10.1016/0022-328X(86)82053-8