反应详情

温度

100 °C

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-ethanone (2.87 g, 9.6 mmol) in DMF (20 mL) was added 5-chlorosalicylaldehyde (1.65 g, 10.5 mmol), potassium carbonate (2.64 g, 19.2 mmol) and potassium iodide (1.59 g, 9.6 mmol). The resulting mixture was heated to 100° C. for 12 hours. The reaction was cooled, diluted with saturated aqueous brine and extracted with ethyl acetate (3×). The combined organics were dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to give crude product. Purification via chromatography on silica gel (15% EtOAc/Hexanes) gave the title compound 3.40 g, 85% yield.)

1. temperatureThe reaction was cooled
2. extractionextracted with ethyl acetate (3×)
3. dry with materialThe combined organics were dried over magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customto give crude product
7. customPurification via chromatography on silica gel (15% EtOAc/Hexanes)