Technology Process of (CO)5WC(OC2H5)NC(C6H4OCH3)2
There total 1 articles about (CO)5WC(OC2H5)NC(C6H4OCH3)2 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
sodium bis(trimethylsilyl)amide;
In
diethyl ether; toluene;
imine in toluene added at -40°C (N2) to NaN(SiMe3)2 in Et2O, stirred (1 h) at room temp., added dropwise to a suspn. of W(CO)6 in Et2O, stirred (1 h), evapd., taken up in CH2Cl2 at -40°C, Et3OBF4 in CH2Cl2 added, warmed to room temp.; solvent was removed, residue extd. with pentane, chromd. on Kieselgel at room temp. (pentane followed by pentane-CH2Cl2), crystd. from pentane,dried for 5 h at room temp. under high vac.; elem. anal.;
DOI:10.1016/0022-328X(85)80071-1
- Guidance literature:
-
With
AlBr3; THF;
In
dichloromethane;
byproducts: AlBr2OEt, AlBr3*THF, CO; further byproduct: (CO)5WCN(C(C6H4OMe)2)2NCW(CO)5; N2 atmosphere; addn.of W-compound in CH2Cl2 to AlBr3 in CH2Cl2 at -10°C; stirring for 30 min; cooling to -40°C; addn. of freshly distilled THF; chromy. (SiO2, pentane/CH2Cl2, CH2Cl2); removal of solvent under high vac.; recrystn. from Et2O; drying at -10°C under high vac. for 1 d; elem. anal.;