反应详情

To a 1 L three-necked flask containing AlCl3 (40 g, 0.299 mol) in 1,2-dichloroethane (600 mL) under N2, butylbenzene (IVe) (49.7 mL, 0.299 mol) was added in one portion at −30° C. To this suspension (4-bromo-phenyl)-acetyl chloride (IIIa) (70 g, 0.299 mol) was added slowly over a period of 30min at such a rate that the internal temperature did not rise above −30° C. The reaction mixture was stirred at this temperature for 45 min and poured into an ice-cold solution of 1.5M HCl (1000 ml). The product was extracted into dichloromethane (2×500 ml), washed with 10% sodium bicarbonate solution (500 ml), water, brine and dried over Na2SO4. The solvent was evaporated under reduced pressure to obtain the titled compound as a white powder (m=90 g) in a 90.9% yield.

1. customdid not rise above −30° C
2. extractionThe product was extracted into dichloromethane (2×500 ml)
3. washwashed with 10% sodium bicarbonate solution (500 ml), water, brine
4. dry with materialdried over Na2SO4
5. customThe solvent was evaporated under reduced pressure