HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium hydroxy sulfite → HCID 70655298, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 70654855 | HCID 70654855 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 70655298 | HCID 70655298 | 100% |
Reaction Steps
To a solution of methyl 6-(4-(3,6-dihydro-2H-thiopyran-4-yl)-2,6-difluorophenyl)-5-fluoropicolinate (1.0 equiv.) in DCM (0.10 M) at rt was added oxone (6.0 equiv.) in one portion. The resulting mixture was stirred at RT overnight, and then refluxed at 40° C. for 4 hrs. 10.0 equiv. of oxone were added and the reaction was allowed to stir at 40° C. over the weekend. The reaction mixture was then diluted with DCM and washed with water the aqueous layer was then separated and extracted with DCM. The combined organic were then dried over MgSO4 and concentrated in vacuo to yield methyl 6-(4-(1,1-dioxido-3,6-dihydro-2H-thiopyran-4-yl)-2,6-difluorophenyl)-5-fluoropicolinate in 100% yield. LC/MS=398.0 (M+H), Rt=0.76 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08987457B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-d69aab5734f34d128ab747a83497e53e |
| Source note | uspto-grants-2015_03 |