反应详情

To a 50 mL three-necked flask containing AlCl3 (4.406 g; 33.05 mmol) under N2, anisole (IVa) (4.467 g; 41.31 mmol) was added in one portion at RT. The reaction was exothermic. To this suspension (4-bromo-phenyl)-acetyl chloride (IIIa) (6.430 g; 27.54 mmol) was added drop wise keeping temperature below 20° C. Then the resulting red suspension was stirred at RT for 3h30. The red thick solution was poured under stirring into a mixture of ice and 1N HCl (100 mL), then the resulting white solid was filtered, and washed with water. The solid was washed with pentane (3×30 mL) and dried under vacuum at RT to give a white powder (m=8.51 g). Purification was performed by crystallization from acetone (30 ml) to give the title compound as a white powder (m=6.113 g) in a 73% yield.

1. customtemperature below 20° C
2. additionThe red thick solution was poured
3. filtrationthe resulting white solid was filtered
4. washwashed with water
5. washThe solid was washed with pentane (3×30 mL)
6. customdried under vacuum at RT
7. customto give a white powder (m=8.51 g)
8. customPurification
9. customwas performed by crystallization from acetone (30 ml)