HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → HCID 86588583, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 22733081 | HCID 22733081 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 86588583 | HCID 86588583 | 66% |
Reaction Steps
To 0.3 g (1.47 mmol) of 1-(2-oxo-2-pyridin-3-yl-ethyl)-pyrrolidin-2-one prepared from Example 20, 0.15 g (2.21 mmol) of hydroxylamine hydrochloride salt and 0.12 g of sodium sulfate were added in methanol/water (1.5:1). The mixture was reacted at 30˜40° C. for 12˜36 hours. Upon completion of the reaction, the reaction mixture was concentrated under reduced pressure, extracted with ethyl acetate for three times, washed with brine for two times, and dried over sodium sulfate. After concentrating under reduced pressure, it was purified by separation with silica gel column chromatography (chloroform/methanol (30:1˜10:1)) to obtain 0.21 g (66% yield) of 1-(2-hydroxyimino-2-pyridin-3-yl-ethyl)-pyrrolidin-2-one as E/Z mixture (1.56:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06716857B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-d9aee380199643a790ed9af95b2ba73c |
| Source note | uspto-grants-2004_04 |