HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium peroxymonosulphate → HCID 71539176, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium peroxymonosulphate | HCID 10313463 | — |
| Reactant | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 89463485 | HCID 89463485 | — |
| Product | HCID 71539176 | HCID 71539176 | 46% |
Reaction Steps
(S)-1-(4-(4-(5-fluoro-2-(methylthio)phenyl)-6-(3-methylmorpholino)-1,3,5-triazin-2-yl)phenyl)-3-methylurea (258 mg, 0.55 mmol) was stirred with Potassium peroxymonosulfate (Oxone) (1.01 g, 1.65 mmol) in THF:MeOH:H2O (5:3:2)(10 ml) for 1 hour at 0° C. Reaction allowed to reach room temperature and stirred overnight with more oxone (1.01 g, 1.65 mmol). The mixture is quenched with saturated sodium thiosulfate solution (10 ml). Diluted with DCM (50 mL) and washed with brine (50 mL). The organic layer was passed through a hydrophobic frit and concentrated in vacuo. The resulting solid was purified by prep HPLC at to afford the title compound as a yellow solid. (127 mg, Yield 46%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09175011B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-3c6a151c9bfd46ecba9494472c22961c |
| Source note | uspto-grants-2015_11 |