HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → (2,4-Difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | (2,4-Difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone | HCID 21960053 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | (2,4-Difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxime | HCID 73856697 | 52% |
Reaction Steps
To the compound (2,4-difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone (22 g) in 95% ethanol (350 ml) and water (100 ml) was added NH2OH.HCl (10.1 g) and ammonium acetate (12.7 g, 2.1 eq). The resulting mixture was refluxed for 3.5 hours. The mixture was then allowed to stir at room temperature for 24 hours. The reaction mixture was concentrated to remove ethanol, poured into water (500 ml), and extracted with dichloromethane (500 ml). This was followed by washing with water, brine, and drying over magnesium sulfate. The product was concentrated to an oil and purified by column chromatography to yield 12 g of (2,4-difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxime.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05811435 |
| Source dataset | uspto-grants-1998_09 |
| ORD ID | ord-a50b807aa12740bb9361038bbc33bd1c |
| Source note | uspto-grants-1998_09 |