反应详情

14.1 g of 1-bis(4-fluorophenyl)methoxy-2-chloroethane, 10.1 g of 4-hydroxypiperidine, 12 g of sodium carbonate and 0.2 g of sodium iodide were added to 200 ml of methyl isobutyl ketone, and the mixture was heated under reflux for 4 hours. At the end of this time, it was filtered, and the solvent was removed by distillation under reduced pressure. The resulting residue was purified by silica gel column chromatography. Elution with a 10:1 by volume mixture of ethanol and methylene chloride afforded 11.5 g (yield 66%) of the title compound as a pale yellow oily substance. p Infrared Absorption Spectrum (CHCl3), νmax cm-1 : 2920, 1600, 1505.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 4 hours
3. filtrationAt the end of this time, it was filtered
4. customthe solvent was removed by distillation under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography
6. washElution with a 10:1
7. additionby volume mixture of ethanol and methylene chloride