HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 10320825, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 9844154 | HCID 9844154 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10320825 | HCID 10320825 | — |
Reaction Steps
To a stirred solution of the sulfide from Example 1 (90 mg, 0.22 mmol) in methanol (2 ml) at 0° C. was added a solution of oxone (205 mg, 0.33 mmol) in water (2 ml). The viscous suspension was further diluted with methanol (2 ml). After 4 hours the reaction mixture was concentrated under reduced pressure and the residue was partitioned between dichloromethane (20 ml) and water (20 ml). The organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude product mixture was purified by flash chromatography on silica gel eluting with pentane:ethyl acetate (50:50, by volume) to give the title compound (70 mg) as a white powder, m.p. 88–90° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07220772B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-bf365ce7fa054c46ab0581a9078bd254 |
| Source note | uspto-grants-2007_05 |