HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 178422879, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 6-Methyl-1H-pyrazolo[3,4-b]pyridine | HCID 55253302 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178422879 | HCID 178422879 | 75% |
Reaction Steps
To a solution of 6-methyl-1H-pyrazolo[3,4-b]pyridine (4.44 g) and iodine (16.9 g) in N,N-dimethylformamide (100 mL) was added potassium hydroxide (7.48 g) under ice-cooling, and the mixture was stirred at room temperature for 4 hours. The reaction solution was poured into ice water, and the precipitate was filtered. The filtrate was extracted with ethyl acetate, washed with saturated saline, and then dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was combined with the above-mentioned precipitate and purified by silica gel column chromatography (eluent: chloroform→chloroform/methanol=19/1) to give 3-iodo-6-methyl-1H-pyrazolo[3,4-b]pyridine [REx(104-2)] (6.48 g) as a brown powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09278944B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-ca5bb403b39e4f6dbcafd9e807ab5f77 |
| Source note | uspto-grants-2016_03 |