Technology Process of OsClI(CS2(CH3))(NO)(P(C6H5)3)2
There total 1 articles about OsClI(CS2(CH3))(NO)(P(C6H5)3)2 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
methyl iodide;
In
dichloromethane;
(N2); addn. of excess CH3I to a suspn. of OsCl(NO)(CS2)PPh3)2, the orange suspn. is stirred for 30 min to give a red soln.; addn. of hexane, evapn. of some solvent with subsequent addns. of hexane (maintaining the vol. in the range of 30-50 ml), filtration, washing (hexane), recrystn. (CH2Cl2/hexane);
DOI:10.1016/S0022-328X(00)99663-3
- Guidance literature:
-
In
ethanol; dichloromethane; water;
(N2); a soln. of OsCl(I)(CS2Me)(NO)(PPh3)2 in CH2Cl2 is treated with a soln. of excess NH4PF6 in water and ethanol, the resulting yellow soln. is stirred for 5 min (if necessary, addn. of ethanol to give a homogeneous soln.); reverse reaction; evapn. of some solvent with intermittent addn. of EtOH (azeotropic removal of CH2Cl2), filtration, washing (EtOH, 2*, hexane, 2*), drying (air); elem. anal.;
DOI:10.1016/S0022-328X(00)99663-3
- Guidance literature:
-
In
tetrahydrofuran; ethanol;
(N2); dropwise addn. of an ethanolic soln. of NaTeH to a soln. of OsCl(I)(CS2Me)(NO)(PPh3)2 in THF at -10°C (ice/ethanol bath), 15 min stirring, warming to room temp. (brown-black suspn.), 20 min stirring, then stirring at air for 5 min; diln. (CH2Cl2), filtration, evapn., extn. (CH2Cl2), chromy. (silica gel, CH2Cl2), 1st pale brown band is collected, evapn., crystn. (CH2Cl2/EtOH), filtration, washing (EtOH, 2*, hexane, 2*), drying in vac.; elem. anal.;
DOI:10.1016/S0022-328X(00)99663-3
