Technology Process of {(p-Cym)OsH(C2H4)PPh3}PF6
There total 1 articles about {(p-Cym)OsH(C2H4)PPh3}PF6 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
tetrahydrofuran;
byproducts: C10H8, NaCl, NaPF6; redn. of {p-CymOsCl(C2H4)PPh3}PF6 suspn. (0.25-0.35 mmol; THF) with NaC10H8 (stirring of C10H8 with excess Na, 12h, THF), -78 °C, addn. of NH4PF6 (0.3-0.4 mmol), -78 °C, slow warming up to room temp., addn. of ether, pptn.; all under N2; decantation, washing of ppt. with ether (3 times), drying (vac.), soln. in CH2Cl2, chromy. (Al2O3), concn., addn. of ether, pptn., filtration, soln. in acetone, chromy. like before, concn., addn. of ether, pptn.; elem. anal.;
DOI:10.1016/0022-328X(88)80244-4
- Guidance literature:
-
In
tetrahydrofuran;
addn. of excess NaH in portions to {(p-Cym)OsH(C2H4)(PPh3)}{PF6} soln. (THF), after end of gas emanation stirring further 5 min; evapn. of solvent (vac.), extn. of residue (pentane); all operations under N2, solvents carefully dried; filtration, concn., cooling to -78 °C;
DOI:10.1016/0022-328X(88)80244-4