HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 89691123, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 89690206 | HCID 89690206 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 89691123 | HCID 89691123 | 78.9% |
Reaction Steps
To a stirred solution of N-(4-bromo-2-(methylamino)phenyl)-3-oxocyclobutanecarboxamide (2.7 g) in CH3CN (20 ml) was added glacial AcOH (2 ml) at room temperature, and then mixture was heated at reflux for 3 h. The mixture was then cooled to room temperature, concentrated in vacuo, and poured into ice-cold saturated NaHCO3 (100 ml). The mixture was extracted with EtOAc, and the extract was washed with water (100 ml) and brine (100 ml), dried over Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (2.0 g) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365540B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-a609134eda2343958aa0b317f90438d1 |
| Source note | uspto-grants-2016_06 |