HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22636403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 22636416 | HCID 22636416 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 22636403 | HCID 22636403 | 58% |
Reaction Steps
To a solution of 2-(4-fluorophenyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-2,3,5,8-tetrahydro-pyrazolo[1,2-a]pyridazin-1-one, 11, (2.4 g, 6.8 mmol) in THF:MeOH (80 mL of 1:1 mixture) is added dropwise a solution of OXONE® (16.8 g, 27.2 mmol) in H2O (80 mL). After stirring 2 hours at room temp, the reaction mixture is diluted with aqueous saturated NaHCO3 and extracted with EtOAc (3×). The combined organic phases are dried, filtered, and concentrated in vacuo to afford 1.5 g (58% yield) of the desired product as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06821971B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-1c2b0247c9db4810a26b4befb29b4571 |
| Source note | uspto-grants-2004_11 |