Technology Process of [ReH(CO)2(P(C6H5)(OC2H5)2)3]
There total 1 articles about [ReH(CO)2(P(C6H5)(OC2H5)2)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 PPh(OEt)2, room temp., ca. 45 h; evapn. (reduced pressure), chromy. (SiO2; light petroleum/Et2O/benzene),evapn. of the 2nd fraction, addn. of EtOH; the byproduct being isolated from the first fraction; 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
- Guidance literature:
-
With
CF3SO3H;
In
tetrahydrofuran; dichloromethane;
byproducts: H2; (Ar or H2); a slight excess of CF3SO3H added to Re complex/CH2Cl2 cooled to -80°C, brought to room temp., stirred for 1 h, excess of LiC2Ph/THF added, stirred for 3 h; solvent removed (vac.), oil treated with EtOH, stirred until solid sepd. out, filtered, dried (vac.);
DOI:10.1016/S0022-328X(00)00020-6