Technology Process of methyltriphenylphosphonium 1,1,1,2,2,2,3,3,4,4-decacarbonyl-3,4-μ-([μ-hydrido-bis(tricarbonylosmio)-Os(Os(3,4))Os'(Os(3,4))])-1,2,3;1,2,4-di-μ3-tricarbonylosmio-tetrahedro-tetraosmate(1-)
There total 1 articles about methyltriphenylphosphonium 1,1,1,2,2,2,3,3,4,4-decacarbonyl-3,4-μ-([μ-hydrido-bis(tricarbonylosmio)-Os(Os(3,4))Os'(Os(3,4))])-1,2,3;1,2,4-di-μ3-tricarbonylosmio-tetrahedro-tetraosmate(1-) which
guide to synthetic route it.
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synthetic route:
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82727-86-4
methyltriphenylphosphonium 1,1,1,2,2,2,3,3,4,4-decacarbonyl-3,4-μ-([μ-hydrido-bis(tricarbonylosmio)-Os(Os(3,4))Os'(Os(3,4))])-1,2,3;1,2,4-di-μ3-tricarbonylosmio-tetrahedro-tetraosmate(1-)
- Guidance literature:
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In
methanol; tert-butyl alcohol;
Os complex refluxed in t-BuOH under N2 for 53 h, evapd. in vac., residue were taken up in acetone, added (MePPh3)Br in MeOH, stirred for 1 h under N2; evapd. in vac., added acetone, filtered ppt. of (Os4H4(CO)12), chromd. (SiO2, acetone/hexane 1:1), (PMePh3)(Os8H(CO)22) recrystd. from CH2Cl2/i-PrOH by slow evapn. techniques;
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82727-86-4
methyltriphenylphosphonium 1,1,1,2,2,2,3,3,4,4-decacarbonyl-3,4-μ-([μ-hydrido-bis(tricarbonylosmio)-Os(Os(3,4))Os'(Os(3,4))])-1,2,3;1,2,4-di-μ3-tricarbonylosmio-tetrahedro-tetraosmate(1-)
- Guidance literature:
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With
KOH;
In
methanol;
to soln. of Os complex in MeOH added excess of KOH in MeOH, kept for 1 h at room temp.; evapd. in vac., added H2O, suspn. filtered through SiO2, solid washed with H2O, removed form SiO2 with CH2Cl2, dried over MgSO4, filtered, concd., (PMePh)Br in MeOH added, slowly evapd. at room temp., ppt. washed with MeOH, pentane;