HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136167197, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 59264794 | HCID 59264794 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 136167197 | HCID 136167197 | 73.9% |
Reaction Steps
Hydroxylamine hydrochloride (75 mg, 1.08 mmol) was added to a suspension of 7-hydroxy-3-(4-methoxy-phenyl)-2-methyl-6-phenyl-chromen-4-one (105 mg, 0.29 mmol) in pyridine (2 ml) and the mixture heated under reflux for ˜6 hrs., to give a pale yellow solution. The solution was allowed to cool and water (20 ml) added. The mixture was extracted with diethyl ether (2×10 ml). The combined extracts were washed with water (2×20 ml) and saturated aqueous sodium chloride solution (10 ml). The solution was dried over anhydrous magnesium sulphate and concentrated. The crude products were purified by column chromatography, silica, eluting with ethyl acetate/hexane (1:1), to give the title compound as an off-white powder (80 mg)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450310B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-7eba0e189cb7408bab9d7d355181baa0 |
| Source note | uspto-grants-2013_05 |