反应详情

温度

100 °C

To a DMF (3 ml) solution of 355 mg of 1-(4-aminophenyl)-4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazine were added 130 mg of 1-chloro-2-(2-chloroethoxy)ethane, 77 mg of sodium iodide and 249 mg of potassium carbonate, followed by overnight stirring at 100° C. After cooled to room temperature, the reaction solution was concentrated under reduced pressure and then water was added thereto, followed by extraction with chloroform. The organic layer was washed with brine and then dried over anhydrous magnesium sulfate, and thereafter, the solvent was evaporated. The residue was purified by silica gel column chromatography (chloroform-methanol) and then crystallization was carried out from ethanol-diethyl ether to obtain 210 mg of 4-(4-{4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazin-1-yl)phenyl)morpholine as yellow crystals.

1. temperatureAfter cooled to room temperature
2. concentrationthe reaction solution was concentrated under reduced pressure
3. additionwater was added
4. extractionfollowed by extraction with chloroform
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was evaporated
8. customThe residue was purified by silica gel column chromatography (chloroform-methanol)
9. customcrystallization