Technology Process of bis(cyclopentadienyliron dicarbonyl) disulfane
There total 1 articles about bis(cyclopentadienyliron dicarbonyl) disulfane which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
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In
tetrahydrofuran;
under N2, THF soln. of Li2S was added slowly to stirred THF soln. of Fe-complex (molar ratio 1:2.42) at room temp., stirred overnight; solvent removed in vac., extd. with Et2O, filtered, reduced in vac., column chromd., eluted with Et2O-petroleum ether and Et2O; identified by (1)H NMR spectra;
- Guidance literature:
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In
diethyl ether;
byproducts: C5H5Fe(CO)2Cl; (Ar); 1.2 equiv. of Et2O soln. of organic ligand added dropwise to Fe-compound in Et2O; stirred for 2 h under protection of light; stripped to dryness; redissolved in CH2Cl2; introduced to silica gel column made up in hexane; eluted with hexane; eluted with Et2O:hexane 1:1 ratio; recrystallized from CH2Cl2/hexane; elem. anal.;
DOI:10.1016/j.poly.2007.04.010
- Guidance literature:
-
With
triphenylphosphine;
In
[(2)H6]acetone;
byproducts: triphenylphosphine sulfide; soln. of Fe-complex and PPh3 (molar ratio 1:2) in acetone-d6 was sealedunder N2; monitored by (1)H NMR spectra;