反应详情

A mixture was prepared by suspending 5.0 g of aluminium chloride into 25 ml of 1,2-dichloroethane. The mixture was added 1.0 ml of acetylchloride, stirred for 1 hour at room temperature. The reaction mixture, wherein 2.4 g of 5-ethyl-2,4'-dimethoxybiphenyl was added, was stirred for 2 hours with cooling by the ice bath and stirred from further 2 hours at room temperature. Ice water was added into the reaction mixture, and extracted with chloroform. The extract was washed with 10% water solution of sodium hydrogencarbonate and an aqueous solution saturated with NaCl, dried with sodium sulfate and concentrated. The concentrate was purified by a silica gel column-chromatography (n-hexane:ethyl acetate=50:1) to yield 1.6 g of 3'-acetyl-5-ethyl-4'-hydroxy-2-methoxybiphenyl.

1. customA mixture was prepared
2. stirringwas stirred for 2 hours
3. stirringstirred from further 2 hours at room temperature
4. extractionextracted with chloroform
5. washThe extract was washed with 10% water solution of sodium hydrogencarbonate
6. dry with materialan aqueous solution saturated with NaCl, dried with sodium sulfate
7. concentrationconcentrated
8. customThe concentrate was purified by a silica gel column-chromatography (n-hexane:ethyl acetate=50:1)