HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → HCID 66876970, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Methyl 3-(4-amino-2-methylphenyl)propanoate | HCID 54187007 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66876970 | HCID 66876970 | 50.7% |
Reaction Steps
A solution of Intermediate 8 (1.4 g) in acetonitrile (20 ml) was added with N-bromosuccinimide (1.4 g, WAKO) under ice cooling, stirred for 10 minutes under ice cooling, and then stirred at room temperature for 3 hours. The reaction mixture was concentrated under reduced pressure, then added with ethyl acetate (10 ml), and successively washed with saturated aqueous ammonium chloride, 5% aqueous sodium sulfite, saturated aqueous sodium hydrogencarbonate and saturated brine, the organic layer was dried, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (Yamazen, n-hexane:ethyl acetate=3:1) to obtain the title compound (1.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08334314B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-094f7a20e4f64cdd8b665e4ef526c289 |
| Source note | uspto-grants-2012_12 |