反应详情

温度

0 °C

A solution of N-(4-methoxyphenyl)-N-(2-methylallyl)acetamide (1.00 g, 4.56 mmol) and aluminium chloride (2.0 g, 15.0 mmol) in 1.0 mL of chlorobenzene was stirred at 110° C. for 3 h. After the reaction mixture was cooled to 0° C., the reaction mixture was diluted with water and ethyl acetate. The separated organic layer was washed with 1 M HCl, saturated NaHCO3 aqueous solution and brine, successively, and dried over MgSO4. After filtration, the filtrate was concentrated in vacuo, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=70/30 to 20/80) to obtain the title compound (0.31 g, 33%), and followed by recrystallization (hexane/ethyl acetate) to obtain the title compound (0.17 g) as a white solid.

1. washThe separated organic layer was washed with 1 M HCl, saturated NaHCO3 aqueous solution and brine
2. dry with materialsuccessively, and dried over MgSO4
3. filtrationAfter filtration
4. concentrationthe filtrate was concentrated in vacuo
5. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=70/30 to 20/80)