Microwave preparation of osmium clusters with anticancer activity; rapid syntheses of Os6(CO)18, Os3(CO)10(acetonitrile)2, and Os3(μ-H)(μ-OH)(CO)10

Microwave-assisted syntheses of the osmium cluster synthons Os6(CO)18, Os3(CO)10(NCMe)2, and Os3(μ-H)(μ-OH)(CO)10 are reported. Microwave irradiation of Os3(CO)12 in a small amount of 1,2-dichlorobenzene is shown to be a superior method of preparing Os6(CO)18 that produces a relatively high yield in only 35 min of heating instead of many days of pyrolysis. In a simple two-step method requiring less than 1 h, the labile complex Os3(CO)10(NCMe)2 is prepared in excellent yield (over 90%). This preparation is accomplished without the need to exclude air from the reaction vessel, and with one-tenth as much solvent and one-half as much trimethylamine-N-oxide as the standard method of synthesis. The cluster Os3(μ-H)(μ-OH)(CO)10 is also conveniently prepared with a small amount of solvent by heating a mixture of Os3(CO)12, silica gel, toluene and water in a microwave reactor for 2 h.

Graphical abstractThe osmium carbonyl cluster complexes Os3(CO)10(acetonitrile)2, Os3(μ-H)(μ-OH)(CO)10, and Os6(CO)18 are rapidly prepared from Os3(CO)12 by microwave irradiation of reaction mixtures with small amounts of solvent in a sealed vessel.Figure optionsDownload full-size imageDownload as PowerPoint slideHighlights► Faster and greener syntheses of osmium clusters by microwave heating. ► Os3(CO)10(acetonitrile)2, Os3(μ-H)(μ-OH)(CO)10, and Os6(CO)18 are efficiently prepared with very small amounts of solvent. ► No inert gases and fewer reagents required.