HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Acetate → (3E)-1-benzyl-3-methoxyimino-5,5-dimethylpyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | 1-Benzyl-5,5-dimethylpyrrolidine-2,3-dione | HCID 66935974 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (3E)-1-benzyl-3-methoxyimino-5,5-dimethylpyrrolidin-2-one | HCID 87210255 | 102.3% |
Reaction Steps
To a solution of 5,5-dimethyl-1-(phenylmethyl)-2,3-pyrrolidinedione (3.9036 g, 17.97 mmol) in MeOH (90 mL) was added sodium acetate (1.81 g, 21.54 mmol) and methoxyamine hydrochloride (1.80 g, 21.55 mmol). The solution was stirred overnight and the solvent was then removed in vacuo. The residue was partitioned between DCM (200 mL), sat. aq. NaHCO3, and water. The aqueous phase was extracted with a fresh portion of DCM (50 mL), and the combined organic phase was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to provide crude (3E)-5,5-dimethyl-1-(phenylmethyl)-2,3-pyrrolidinedione 3-(O-methyloxime) (4.5282 g, >100% crude yield) as a yellow/orange oil. LCMS: (M+H)+: 247.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07893056B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-70e26ca5a25542a39aed0f086cce7492 |
| Source note | uspto-grants-2011_02 |