反应详情

To a stirring solution of 1-(3-bromo-phenyl)-pentane-1,4-dione (18.32 mmol) in toluene (90 mL) was added Lawesson's Reagent (19.24 mmol, 1.05 eq.) and the mixture was heated to reflux for 20 min. The reaction mixture was then cooled to room temperature and diluted with 1:1 hexanes/ether (90 mL) resulting in a precipitate. The mixture was filtered through a small pad of celite and the filtrate was concentrated to a light yellow solid that was purified by recrystallization from hexanes to give the final product as a white solid (12.17 mmol, 66%). MS (ESI) m/z 254.3.

1. temperaturethe mixture was heated
2. temperatureto reflux for 20 min
3. customresulting in a precipitate
4. filtrationThe mixture was filtered through a small pad of celite
5. concentrationthe filtrate was concentrated to a light yellow solid
6. customthat was purified by recrystallization from hexanes