反应详情

To a stirred mixture of piperidine-4-carboxylic acid [6-(2-ethoxy-phenyl)-pyrimidin-4-yl]-amide (compound #1A) (0.25 g, 0.76 mmol) and NEt3 (0.01 mL, 0.76 mmol) in THF (10 ml) was added acetyl chloride (0.053 ml, 0.76 mmol) at 0° C. The mixture was stirred at room temperature for 20 min, then the solvent was distilled off; the residue was dissolved in water and extracted with ethyl acetate (3×10 ml). The organic layers were separated, combined, dried over sodium sulfate, filtered and concentrated under reduced pressure. The resulting crude product was triturated with dry diethyl ether and the solid was filtered off to obtain 1-acetyl-piperidine-4-carboxylic acid [6-(2-ethoxy-phenyl)-pyrimidin-4-yl]-amide (compound #13A) (0.208 g, 73%) as a white solid.

1. distillationthe solvent was distilled off
2. dissolutionthe residue was dissolved in water
3. extractionextracted with ethyl acetate (3×10 ml)
4. customThe organic layers were separated
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe resulting crude product was triturated with dry diethyl ether
9. filtrationthe solid was filtered off