HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxybromide → HCID 178468568, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | HCID 178469360 | HCID 178469360 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178468568 | HCID 178468568 | 68.5% |
Reaction Steps
Ethyl 3-ethyl-6-hydroxy-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (0.52 g, 2.21 mmol) was suspended in acetonitrile (6 mL) and POBr3 (1.27 g, 4.42 mmol) was added to it. The reaction mixture was refluxed for 6 h. On completion of reaction, acetonitrile was removed under reduced pressure and residue neutralized with saturated NaHCO3. Extraction was carried out using EtOAc; the combined organic layers were washed with water, brine and dried over anhydrous Na2SO4; filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to provide the desired intermediate (0.45 g, 68.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598167B1 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-3bc665cb189f4fcbb4e6c566595112c4 |
| Source note | uspto-grants-2013_12 |