Methane → HCID 59497122, compound

Participants

Reaction Steps

A solution of SeO2 (2.18 g, 19.6 mmol) in a mixture of dioxane (100 mL) and water (4 mL) was heated to reflux in a two-neck 250 mL round-bottomed flask. A solution of 2-methyl-4-methylsulfanyl-[1,10]phenanthroline (1.89 g, 7.90 mmol) in hot dioxane (100 mL) was added through an addition funnel over a period of 1 hour and the reaction mixture was refluxed for additional 45 minutes. The reaction mixture was filtered while hot and the residue rinsed with more hot dioxane (20 mL) and filtered. The filtrate was concentrated in vacuo and the residue obtained was redissolved in hot water, stirred with decolorizing charcoal and filtered. The filtrate was allowed to reach room temperature and basified with saturated NaHCO3 until precipitation of a white solid, which was filtered, washed with cold water and dried in vacuo. A white solid (0.80 g, 41% yield) was obtained.

Provenance & Evidence