반응 #61971

ord-954f43423d5043489dc3b51ea2e8b455

반응 조건

온도
105°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool to room temperature
  2. 2
    추출extracted with methylene chloride (2×20 mL)
  3. 3
    건조The combined organic phases were dried (magnesium sulfate)
  4. 4
    기타evaporated in vacuo
  5. 5
    workup.DISTILLATIONKugelrohr distillation of the residue (5 mm Hg, 260° C.)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07429586B2uspto-grants-2008_09