反应详情

In an oven-dried flask placed under a nitrogen atmosphere biphenyl (50 g) was stirred in dichloromethane (450 mL). The flask was placed in an ice bath and to it was added benzoyl chloride (46 mL) via addition funnel slowly over 20 minutes. To that mixture was added anhydrous aluminum chloride (51 g) via solid addition funnel, slowly over 10 minutes. After the aluminum chloride addition was complete the reaction mixture allowed to warm to room temperature and to stir for 16 hours. The reaction mixture was slowly poured into a beaker containing ice and a 10% aqueous solution of hydrochloric acid (600 mL) while stirring vigorously. A separatory funnel was used to separate the organic and aqueous layers. The recovered organic layer was then washed with water (2×500 mL), washed with a saturated aqueous solution of sodium chloride (500 mL), dried over sodium sulfate and concentrated by rotary evaporation. The resulting solid was slurried in a 25% v/v mixture of ethyl acetate in hexanes. The solid was collected by vacuum filtration, and then washed with cold diethyl ether (2×200 mL) to yield 57 g of [1,1′-biphenyl]-4-yl(phenyl)methanone.

1. customIn an oven-dried flask placed under a nitrogen atmosphere
2. customThe flask was placed in an ice bath and to it
3. additionvia addition funnel slowly over 20 minutes
4. additionvia solid addition funnel
5. additionThe reaction mixture was slowly poured into a beaker
6. additioncontaining ice
7. customA separatory funnel was used
8. customto separate the organic and aqueous layers
9. washThe recovered organic layer was then washed with water (2×500 mL)
10. washwashed with a saturated aqueous solution of sodium chloride (500 mL)
11. dry with materialdried over sodium sulfate
12. concentrationconcentrated by rotary evaporation
13. additionThe resulting solid was slurried in a 25% v/v mixture of ethyl acetate in hexanes
14. filtrationThe solid was collected by vacuum filtration
15. washwashed with cold diethyl ether (2×200 mL)