HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 69217838, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Potassium peroxymonosulphate | HCID 10313463 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 59643065 | HCID 59643065 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69217838 | HCID 69217838 | — |
Reaction Steps
To a solution of [7-(2,6-difluoro-phenyl)-2-methylsulfanyl-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-(4-fluoro-phenyl)-methanone, 3, (4.6 g, 11.5 mmol) in THF:methanol (108 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (28.4 g, 46.1 mmol) in H2O (83 mL). After stirring the reaction for 1 hour at room temperature, the solution is poured into aqueous saturated NaHCO3. The aqueous phase is extracted three times with EtOAc and the combined organic phases are dried (MgSO4), filtered and concentrated in vacuo to afford 4.5 g of the desired product which is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07319102B1 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-afe7c2ebba0a4001a35201e4c15106c3 |
| Source note | uspto-grants-2008_01 |