Technology Process of butane, tungsten
There total 4 articles about butane, tungsten which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
tetrahydrofuran; diethyl ether;
byproducts: MgCl2; WCl6 in Et2O was reacted with Mg-complex suspd. in THF under N2, dioxane was added; filtered, solvent was evapd., residue was dissolved in toluene, eluted down a silica column, eluent was evapd., recrystd. from hexane;
- Guidance literature:
-
With
iodine; magnesium; ethyl iodide;
In
tetrahydrofuran;
Mg with I2 heated in vac., activated by EtI, suspended in THF, added W-complex and ligand butadiene at -20°C, stirred for 48 h, at -20- -15°C; solvent evapd. at -10°C, residue dried at 25°C in vac., extractd. with toluene, then with pentane , row product dissolved THF at 50°C, stand at -20°C, added ether, filtered, dried in vac.;
- Guidance literature:
-
With
magnesium anthracene;
In
tetrahydrofuran;
under Ar; WCl6 slowly added to cooled (-78°C) and stirred soln. of magnesium-anthracene (prepared in situ from Mg, anthracene, CH3I in THF), the diene siphoned into flask, mixt. allowed to warm very slowly toroom temp., stirred for 24 h; evapn. of volatiles (vac.), residue extd. (pentane), evapn., sublimation (120°C, 10**-4 torr), crystn. (THF), elem. anal.;
DOI:10.1016/0022-328X(86)84009-8
