HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 178468692, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Reactant | CID 59797354 | HCID 59797354 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178468692 | HCID 178468692 | 80.4% |
Reaction Steps
To 15 mL of a solution of 1.33 g of 4-methoxy-1H-indazole-5-carboxylic acid ethyl ester in N,N-dimethylformamide were added 1.95 g of iodine and 0.85 g of potassium hydroxide, stirred at room temperature for 1 hour and 40 minutes, added with another 0.8 g of iodine, and stirred for 3 hours and 20 minutes. Thereafter, 10% sodium hydrogen sulfite aqueous solution was added, extracted twice with ethyl acetate, and the organic layer was washed once with saturated brine, dried over magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography, to afford 1.68 g of the title compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07429609B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-76b38609be7a41c29b6c85e3479acf20 |
| Source note | uspto-grants-2008_09 |