HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 54476165, compound → HCID 66645913, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 54476165 | HCID 54476165 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 66645913 | HCID 66645913 | 65.5% |
Reaction Steps
5% palladium carbon (1.5 g) were added to an ethanol solution (250 ml) of ethyl 2-(4-methoxy-2-nitrophenoxy)-2-methylpropionate (14.6 g, 51.6 mmol) to perform catalytic reduction at room temperature. The catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. Water was added to the obtained residue, which was then extracted with ethyl acetate. The extraction solution was dried over magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=9:1). The purified product was concentrated to dryness under reduced pressure to obtain 6-methoxy-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (7.0 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071600B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-2913df16b10841aaa446cb4978ef6e3a |
| Source note | uspto-grants-2011_12 |