HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 178468567, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | HCID 178434478 | HCID 178434478 | — |
| Product | HCID 178468567 | HCID 178468567 | 77.8% |
Reaction Steps
6-Hydroxy-3-methyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (2.5 g, 11.3 mmol) was suspended in acetonitrile (25 mL) and POBr3 (6.5 g, 22.6 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 and 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 target compound (2.5 g, 77.8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962620B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-491c7b06fa894a799369c6dc97064fa5 |
| Source note | uspto-grants-2015_02 |