反応 #1605824

ord-2799d29ec068457bae7f754eba4eea3a

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was heated
  2. 2
    温度under reflux for 18 hours
  3. 3
    ろ過The reaction solution was filtered
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    workup.ADDITIONdiluted with ethyl acetate
  6. 6
    洗浄The organic layer was washed with a saturated aqueous solution of sodium chloride
  7. 7
    乾燥dried over anhydrous magnesium sulfate
  8. 8
    濃縮concentrated under reduced pressure
  9. 9
    その他The residue was purified by flash column chromatography

実験手順

To a solution of sodium ethoxide (3.5 g, 50 mmol) in ethanol (100 mL), 1-(chloromethyl)-4-nitrobenzene (8.6 g, 50 mmol) and 2-nitropropane (2.2 g, 250 mmol) were added at room temperature, and the mixture was heated under reflux for 18 hours. The reaction solution was filtered, concentrated under reduced pressure, and diluted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by flash column chromatography to obtain 1-(2-methyl-2-nitropropyl)-4-nitrobenzene (8.52 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09072734B2uspto-grants-2015_07