Technology Process of (CO)3(P(CH3)3)2Re(OC6H4CH3)
There total 2 articles about (CO)3(P(CH3)3)2Re(OC6H4CH3) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
KN(Si(CH3)3)2;
In
tetrahydrofuran;
mixing of p-cresol and KN(TMS)2; addn. of THF; stirring at room temperature for 20 min; addn. to Re-compound; stirring for 2 days at room temperature; inert atm.;; removal of volatiles under vac.; dissolving in toluene; filtration; removal of toluene in vac.;;
DOI:10.1021/om00027a031
- Guidance literature:
-
In
benzene;
byproducts: P(C6H5)3; charging a bomb with Re-compound in C6H6; condensation of P(CH3)3 into the bomb at -196°C; heating to 45°C overnight; inert atm.;; concn.; pptn. by addn. of hexanes; filtration; washing with hexane; dissolving in toluene; layering with pentane; cooling to -40°C overnight; crystallization; filtration; washing with hexane; drying in high vac. for 12 h; elem. anal.;;
DOI:10.1021/om00027a031
- Guidance literature:
-
With
CS2;
In
benzene;
bomb charged with Re-compd. and solvent in a drybox, CS2 condensed into the bomb, heated for 7 days at 140°C, color changed, cooled to room temp;; monitored by 31P-NMR, evapd. (vac.), dissolved in toluene, diffusion of pentane vapor into soln. at room temp., crystn. within 4 days, washed (pentane), dried ; elem. anal.;