反应详情

135 ml (135 mmole) of a solution of phenylmagnesium bromide (1M) in THF was added to a hot suspension of 6-phenylpyridazinone compound 7.8 g (45 mmole) in dry toluene (50 ml). The mixture was refluxed for 8 h, left overnight at ambient temperature, then decomposed with a saturated solution of ammonium chloride. The organic layer was separated, and the aqueous layer was extracted with 100 ml of ethyl acetate. The solvent was removed and the residue was crystallized from ethanol. The crystals were collected by filtering and dried over a medium frit sintered glass funnel in vacuo to give 5.6 g of white crystals. Yield was 50%, confirmed by ESI-MS, ESI-MS: m/z 250.1 (M+H+).

1. temperatureThe mixture was refluxed for 8 h
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with 100 ml of ethyl acetate
4. customThe solvent was removed
5. customthe residue was crystallized from ethanol
6. customThe crystals were collected
7. filtrationby filtering
8. customdried over a medium frit sintered glass funnel in vacuo