Technology Process of 9-phenylethynyl-1,2-dicarba-closo-dodecaborane(12)
There total 2 articles about 9-phenylethynyl-1,2-dicarba-closo-dodecaborane(12) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
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tetrakis(triphenylphosphine) palladium(0);
In
1,4-dioxane; diethyl ether;
addn. of EtMgBr in ether to a soln. of acetylenic derivate in absolute dioxane (N2), heating for 1 h at 40°C, cooling, addn. of carborane and Pd-catalyst in dioxane, heating for 40 h at 60°C (stirring), monitoring of react. by GLC; pouring into a ca. 18% soln. of HCl, extn. by ether, washing with H2O, drying (MgSO4), distn. of solvents in vac., column chromy. of residue (silica gel), benzene-petroleum ether (bp 40-70°C) as eluent; elem.anal.;
DOI:10.1007/BF00948065
- Guidance literature:
-
With
n-butyllithium;
tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran; hexane;
dry Ar; CHC(C4H9) in THF and n-C4H9Li in hexane stirred 30 min; ZnCl2 in THF added; mixt. stirred 30 min; reflux with iodocarborane and catalyst (30, 30, 30, 10, 0.2 mmol) for 8 h; poured into HCl; extd. aq. layer (ether); org. fractions combined; dried (Na2SO4); filtered; solvent removed; column chromy. (silica gel, benzene-heptane (1:4));