反应详情

温度

90 °C

Mix (benzo[b]thiophene-3-yl)(4-piperidinyl)methanone.CF3CO2H (2.0 g, 5.56 mmol), 2-(4-methoxyphenyl)ethyl bromide (1.27 g, 5.93 mmol), potassium carbonate (1.95 g, 1.41 mmol) and anhydrous dimethylformamide (20 mL). Warm to approximately 90° C. and stir overnight. Allow to cool to room temperature and partition between a 2:1 mixture of ethyl acetate:toluene and water. Separate the aqueous phase and wash the organic phase with water and saturated sodium chloride. Dry (Na2SO4) and evaporate the solvent in vacuo. Purify by chromatography (40% ethyl acetate/hexane) and recrystallize (cyclohexane) to give the title compound as pale yellow plates; mp 114°-116° C.

1. temperatureto cool to room temperature
2. custompartition between a 2:1 mixture of ethyl acetate
3. customSeparate the aqueous phase
4. washwash the organic phase with water and saturated sodium chloride
5. dry with materialDry (Na2SO4)
6. customevaporate the solvent in vacuo
7. customPurify by chromatography (40% ethyl acetate/hexane)
8. customrecrystallize (cyclohexane)