HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86751350, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 10680936 | HCID 10680936 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86751350 | HCID 86751350 | 43% |
Reaction Steps
A mixture of 7-tert-butyl-5-cyano-2,3-dihydro-3,3-dimethylbenzo[b]furan (6.39 g, 27.9 mmol), potassium carbonate (15.80 g, 114.0 mmol), hydroxylamine hydrochloride (7.93 g, 114.0 mmol), and 135 mL of ethanol is heated at reflux for 20 h. The reaction mixture is cooled to room temperature, filtered, and concentrated in vacuo to give a solid residue. Purification by flash column chromatography on silica gel (20% ethyl acetate-hexane→5% methanol-dichloromethane) furnishes about 3.13 g (43%) of the title compound as a colorless foamy solid: mp 109°-110 ° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05821250 |
| Source dataset | uspto-grants-1998_10 |
| ORD ID | ord-94b2ead83c62405aa617dcb000dd8a7a |
| Source note | uspto-grants-1998_10 |