HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21252829, compound → HCID 21252814, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21252829 | HCID 21252829 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 21252814 | HCID 21252814 | 2% |
Reaction Steps
6-chloro-1-(4-chlorophenyl)-4(1H)-quinolinone (2 g) obtained in step 4 was dissolved in acetic acid (150 ml) and to the solution were added a boron tribromide-acetic acid complex (44 ml) and palladium diacetate (6.28 g). The mixture was heated under reflux for 1 hour in an argon atmosphere and allowed to cool. The insoluble content was removed by filtration and the solution was extracted with water and ethyl acetate. The ethyl acetate layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel flash column chromatography (eluent: hexane/ethyl acetate=1:2) to obtain the title compound (40 mg, 2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06018046 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-285712732b6e4d89bf68867c8a37b76d |
| Source note | uspto-grants-2000_01 |