反应详情

温度

60 °C

A mixture of N-[3-(4-aminophenyl)propyl]-5-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4-amine (0.014 g, 0.037 mmol) and acetic anhydride (0.01 mL) in methylene chloride (2.0 mL) was heated to 60° C. for 6 h. The reaction was allowed to cool to room temperature and concentrated in vacuo. The residue was then dissolved in ethyl acetate (30 mL) and the organic layer was washed with sodium bicarbonate (2×25 mL). Concentration, followed by followed by silica gel column chromatography purification (using 3% methanol in 1:1 ethyl acetate/hexane and ammonia (0.03%) as eluent) afforded N-[4-(3-{[5-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4-yl]amino}propyl)phenyl]acetamide in 90% yield.

1. temperatureto cool to room temperature
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was then dissolved in ethyl acetate (30 mL)
4. washthe organic layer was washed with sodium bicarbonate (2×25 mL)
5. concentrationConcentration
6. customby followed by silica gel column chromatography purification (using 3% methanol in 1:1 ethyl acetate/hexane and ammonia (0.03%) as eluent)