反应详情

温度

85 °C

To a dimethylsulfoxide (4.0 mL) solution of 0.26 g of 2-fluoro-4-[3-(4-piperidinyl)propoxy]benzonitrile and 0.21 g of 4-(3-chloropropoxy)-2-fluorobenzonitrile was added 0.88 mL of N-ethyldiisopropylamine, which was then stirred at 80 to 90° C. for 8 hours and 15 minutes. The reaction mixture was cooled down to room temperature, to which water was then added, followed by extraction with ethyl acetate. The extract was washed twice with water and dried with anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The resultant residue was purified using silica gel column chromatography (eluent; chloroform:methanol=10:1) to provide 0.25 g of 4-(3-{1-[3-(4-cyano-3-fluorophenoxy) propyl]-4-piperidinyl}propoxy)-2-fluorobenzonitrile as brown solid form.

1. additionwas then added
2. extractionfollowed by extraction with ethyl acetate
3. washThe extract was washed twice with water
4. dry with materialdried with anhydrous magnesium sulfate
5. distillationby distilling off the solvent under reduced pressure
6. customThe resultant residue was purified