Technology Process of [W(CO)5CPh(C6H4-p-OCH3)]
There total 2 articles about [W(CO)5CPh(C6H4-p-OCH3)] which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
diethyl ether;
under N2, soln. of W complex in Et2O cooled to -78°C, 0.32 M soln. of LiC6H4OMe in Et2O added dropwise, stirred at -78°C for 1 h before addn. of 0.43 M HCl in Et2O at -78°C, after 45 min warmed slowly to 0°C, SiO2 added; evapd. in vac., chromd. (SiO2, pentane-Et2O, -15°C), collected at 0°C, concd. in vac., cooled to -78°C; elem. anal.;
DOI:10.1021/ja00321a018
- Guidance literature:
-
In
cyclohexane;
Irradiation (UV/VIS); under N2, soln. of W(CO)5CPh2 in C6H12 added to soln. of alkene in C6H12, irradiated through Pyrex filter at 25.+-.1°C for 4 h / kinetics monitored at 12-14 and 27-29°C by UV; concd. in vac., extd. with cold pentane (-10°C), evapd., redissolved in CCl4, chromd. (SiO2/deactivated with H2O, CCl4, -15°C), collected at 0°C, evapd. in vac., dissolved in pentane, evapd. in vac.; elem. anal.;
Kinetics;
DOI:10.1021/ja00321a018
- Guidance literature:
-
In
diethyl ether;
addn. of PhNCSe to W-complex in Et2O at -30°C under N2, stirringfor 1 h at this temp., colour changes from deep red to dark blue; chromy. (SiO2, -25°C), elution (pentane and pentane/Et2O), deep blue band, evapn. of solvent in high vaccum, dissolution (pentane, -20°C), chromy. (SiO2, -25°C), evapn. of solvent in high vac., recrystn. from pentane, elem. anal.;
