HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 178505545, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 4,6-Bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine | HCID 11961374 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 178505545 | HCID 178505545 | 97% |
Reaction Steps
To a suspension of 4,6-bis(4-fluorophenyl)-5-(4-pyridyl)-1H-pyrazolo[3,4-b]pyridine (1.00 g, 2.6 mmol, obtained in example 1) in CHCl3 (10 mL), a solution of Br2 (0.69 g, 4.3 mmol) in CHCl3 (3 mL) was added under argon atmosphere. Acetonitrile (4 mL) was added and the mixture was stirred at room temperature for 2 days. The residue was concentrated, dissolved in CHCl3 and washed with 1 N NaOH. A precipitate was formed, which was filtered and dissolved with MeOH. The solution was concentrated and washed with 1 N NaOH. It was extracted with EtOAc, dried over Na2SO4 and concentrated. This was treated with diethyl ether, the solvent was decanted and the product obtained was dried to afford 1.16 g of the title compound (yield: 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07468376B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-3bdedd9339fb4715ba7b7c6fa7f32ed5 |
| Source note | uspto-grants-2008_12 |