HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → HCID 178509237, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Potassium hydroxy sulfite | HCID 23707502 | — |
| Edukt | HCID 178509236 | HCID 178509236 | — |
| Produkt | HCID 178509237 | HCID 178509237 | 81% |
Reaktionsschritte
A solution of 663 mg (1.078 mmol) of oxone in 1.1 ml of water is added to a solution of 300 mg (1.078 mmol) of 5-(3,5-difluorophenylthio)-1H-pyrazolo[3,4-b]pyridin-3-amine in 10 ml of a 1:1 mixture of tetrahydrofuran and methanol at 0° C. The reaction mixture is stirred at room temperature for 16 hours. An additional portion of 663 mg of oxone at 0° C. is then added and the reaction medium stirred at room temperature for 24 hours. The solvents are evaporated and the reaction medium is diluted with sodium bicarbonate solution, extracted with ethyl acetate, dried on MgSO4 and then concentrated to yield 340 mg (81%) of 5-(3,5-difluorophenylsulfonyl)-1H-pyrazolo[3,4-b]pyridin-3-amine in the form of a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09381195B2 |
| Quelldatensatz | uspto-grants-2016_07 |
| ORD ID | ord-e1bb9da3e2bc4b77912e8f432323058a |
| Quellennotiz | uspto-grants-2016_07 |