反応 #61971

ord-954f43423d5043489dc3b51ea2e8b455

反応条件

温度
105°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    抽出extracted with methylene chloride (2×20 mL)
  3. 3
    乾燥The combined organic phases were dried (magnesium sulfate)
  4. 4
    その他evaporated in vacuo
  5. 5
    workup.DISTILLATIONKugelrohr distillation of the residue (5 mm Hg, 260° C.)

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07429586B2uspto-grants-2008_09