HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → 1-(4-Iodo-pyrazolo[3,4-b]pyridin-1-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | 4-Chloro-1H-pyrazolo[3,4-b]pyridine | HCID 310045 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-(4-Iodo-pyrazolo[3,4-b]pyridin-1-yl)ethanone | HCID 21877400 | 42% |
Reaction Steps
A mixture of 4-chloro-1H-pyrazolo[3,4-b]pyridine (820 mg, 5.30 mmol), sodium iodide (2.4 mg, 16.0 mmol), and acetyl chloride (0.8 ml) in acetonitrile (6 ml) was refluxed 8 h. The mixture was then treated with a 10% aqueous solution of NaCO3 (10 ml), and a 10% aqueous solution of NaHSO3 (10 ml), and held 10 min. The mixture was extracted with ethyl acetate (50 ml), and the organics were washed with brine (10 ml), dried over MgSO4, and evaporated under reduced pressure. Purification by silica gel chromatography gave 1-(4-iodo-pyrazolo[3,4-b]pyridin-1-yl)-ethanone as a brown solid (650 mg, 42%). 1H NMR (300 MHz, CDCl3) δ 8.39 (d, 1H, J=5.0 Hz), 8.04 (s, 1H), 7.76 (d, 1H, J=5.0 Hz), 2.88 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07141587B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-5c5e4f82afa14fedaf5fb02f98d54cdd |
| Source note | uspto-grants-2006_11 |