反应详情

温度

0 °C

To a solution of 4-cyanophenol (5.95 g, 0.05 mol) in DMF (35 mL) at 0° C. was added 60% NaH (2.2 g, 0.055 mol). The reaction mixture was stirred at 0° C. for 15 minutes, then at room temperature for 15 minutes and then N-(2-chloroethyl)morpholine (prepared from 11.16 g, 0.06 mol of the hydrochloride salt) was added and the reaction mixture was stirred at room temperature for about 2 days. There was still a small amount of starting material present so the reaction mixture was heated on a steam bath for 4 hours. The reaction mixture was cooled to room temperature and then the solvent was removed. Ice-water was added to the residue and the solid which precipitated was collected by filtration and dried to afford 11.3 g (97%) of 4-[2-(4-morpholinyl)ethoxy]benzonitrile.

1. waitat room temperature for 15 minutes
2. additionwas added
3. stirringthe reaction mixture was stirred at room temperature for about 2 days
4. temperaturewas heated on a steam bath for 4 hours
5. temperatureThe reaction mixture was cooled to room temperature
6. customthe solvent was removed
7. additionIce-water was added to the residue
8. customthe solid which precipitated
9. filtrationwas collected by filtration
10. customdried