反应详情

温度

172 °C

Under argon gas, a suspension of 2-bromomethyl-2,3-dihydro-2,4,6,7-tetramethyl-5-benzofuranamine (1.4 g), N-[bis(4-fluorophenyl)methyl]-4-piperidinamine (4.5 g), and potassium carbonate (1.4 g) in N,N-dimethylacetamide (20 mL) was stirred at 172° C. for 4.5 hours. This reaction mixture was diluted with water and extracted with ethyl acetate. The extract was washed with water and saturated aqueous sodium chloride solution, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by column chromatograph (silica gel/ethyl acetate and basic silica gel/hexane:ethyl acetate=9:1-85:15) and recrystallized from ethyl acetate-hexane to provide the title compound (0.97 g, yield 39%).

1. extractionextracted with ethyl acetate
2. washThe extract was washed with water and saturated aqueous sodium chloride solution
3. dry with materialdried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatograph (silica gel/ethyl acetate and basic silica gel/hexane:ethyl acetate=9:1-85:15)
6. customrecrystallized from ethyl acetate-hexane