Reaktion #61971
ord-954f43423d5043489dc3b51ea2e8b455
Reaktionsgleichung
Reaktionsbedingungen
Temperatur
105°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturto cool to room temperature
- 2Extraktionextracted with methylene chloride (2×20 mL)
- 3TrocknenThe combined organic phases were dried (magnesium sulfate)
- 4Sonstigeevaporated in vacuo
- 5workup.DISTILLATIONKugelrohr distillation of the residue (5 mm Hg, 260° C.)
Vorschrift
A suspension of 4-(3-chloro-1-propoxy)iodobenzene (5 g), piperidine (2.2 mL), sodium carbonate (2.7 g), and potassium iodide (140 mg) in n-butanol (30 mL) was heated in a 105° C. bath for 18 h. The resulting mixture was allowed to cool to room temperature, diluted with water (50 mL), and extracted with methylene chloride (2×20 mL). The combined organic phases were dried (magnesium sulfate), and evaporated in vacuo. Kugelrohr distillation of the residue (5 mm Hg, 260° C.) gave the title compound as a white crystalline solid (4.8 g).