Methane → HCID 59497122, compound

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.

1. temperaturewas heated
2. temperatureto reflux in a two-neck 250 mL round-bottomed flask
3. temperaturethe reaction mixture was refluxed for additional 45 minutes
4. filtrationThe reaction mixture was filtered while hot and the residue
5. washrinsed with more hot dioxane (20 mL)
6. filtrationfiltered
7. concentrationThe filtrate was concentrated in vacuo
8. customthe residue obtained
9. filtrationfiltered
10. customto reach room temperature and basified with saturated NaHCO3 until precipitation of a white solid, which
11. filtrationwas filtered
12. washwashed with cold water
13. customdried in vacuo

ORD record

ord-8d1681434c2e43a59c439dd81921655e

Source dataset

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08592446B2