Technology Process of Re(hydride)(carbonyl)2(PPh2(OEt))3
There total 1 articles about Re(hydride)(carbonyl)2(PPh2(OEt))3 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
toluene;
Irradiation (UV/VIS); (argon); irradiation (Pyrex Schlenk flask, 400 W mercury arc lamp), excess PPh2(OEt), room temp., ca. 45 h; evapn. (reduced pressure), chromy. (SiO2; light petroleum/Et2O/benzene),evapn. of the 2nd fraction, addn. of EtOH; traces of the byproduct bein g isolated from the first fraction; elem. anal.;
- Guidance literature:
-
With
HBF4*OEt2;
In
ethanol;
(argon); addn. of HBF4*OEt2 to the Re complex in EtOH at -80°C, warming to room temp., stirring (2 h), addn. of excess NaBPh4 in EtOH; filtration, crystn. (CH2Cl2/EtOH); elem. anal.;
- Guidance literature:
-
With
HBF4*(C2H5)2O; (C2H5)3N;
In
diethyl ether; dichloromethane;
byproducts: H2; (Ar or H2); a slight excess of HBF4*Et2O/Et2O added to Re complex/CH2Cl2 cooled to -80°C, brought to room temp., stirred for 1 h, excessof PhC2H added, stirred for 3-4 h, excess of Et3N added, stirred for 3 h; solvent removed (vac.), oil extd. (C6H6), solvent evapd., oil triturated with EtOH until solid sepd. out, filtered, dried (vac.); elem. anal.;
DOI:10.1016/S0022-328X(00)00020-6