HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 4-Bromo-1H-indole-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 4-bromo-1H-indole-2-carboxamide | HCID 59151273 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-Bromo-1H-indole-2-carbonitrile | HCID 59151301 | 82.3% |
Reaction Steps
Phosphorous oxychloride (1.9 mL, 20 mmol) was added to a suspension of 4-bromo-1H-indole-2-carboxylic acid amide (1.32 g, 5.5 mmol.) in toluene (10 mL) and the mixture was stirred at reflux for 45 min. On cooling, the mixture was poured into an aqueous Na2CO3 solution (sat., 50 mL) and the mixture stirred until effervescence had subsided. The layers were separated, the aqueous phase extracted with EtOAc and the combined organic layers dried (MgSO4) and evaporated to dryness. The crude material was purified by column chromatography to afford the title compound as a solid (1.00 g, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697693B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-6ddc06bd0bf048cbac98276d23aa3f70 |
| Source note | uspto-grants-2014_04 |