Technology Process of Digermane, pentaphenyl-
There total 1 articles about Digermane, pentaphenyl- which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
tetrahydrofuran;
Ph2ClGeH was added to Ph3GeLi (prepd. from Ph3GeH and BuLi) in THF under Ar, mixt. was heated under reflux (65°C) for 2 h; reaction mixt. was hydrolyzed, extd. with ether. ext. dried over Na2SO4, concd. under reduced pressure, residue was recrystd. from ethanol/ether; elem. anal.;
DOI:10.1016/S0022-328X(00)98750-3
- Guidance literature:
-
With
2,2'-azobis(isobutyronitrile);
In
neat (no solvent);
Ge deriv. heating with an excess of disulfide and a catalytic amt. of AIBN in a sealed tube for 12 h at 100°C, volatiles removing in vacuo, white crystalline residue washing with pentane; identified by elem. anal. and NMR spectrum;
DOI:10.1016/0022-328X(84)85145-1
- Guidance literature:
-
With
n-BuLi;
In
diethyl ether;
byproducts: Ge2Ph6, Ge3Ph8, n-Ge4Ph10; under Ar; HGe2Ph5 suspensed in Et2O at 0°C; n-BuLi added during 5 min; stirred 15 min at room temperature; solution was dropped to GePh2Cl2 at -65°C during 2 h; warmed to room temperature; NH4Cl added;; evaporated to dryness; dissolved in CH2Cl2; chromatographed; eluent: n-heptane/CH2Cl2 92/8; last fraction evaporated, dissolved in CH2Cl2 and CH3CN; crystals after a few days; recrystallization from CH2Cl2/CH3CN; elem. anal.;
DOI:10.1016/0022-328X(86)82075-7
