反応 #4217

ord-81dc0c6c46c04f688c9e0a0ed9716418

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture heated
  2. 2
    温度to reflux for 30 hours
  3. 3
    乾燥dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONThe residue was distilled under vacuum

実験手順

Aniline, (102.3 g, 1.1 mole) was added to 50 ml of dioxane, 108 g of 1,2-epoxy butane and 1 g of potassium fluoride in 25 ml of water. The mixture heated to reflux for 30 hours. The mixture was poured into water, taken up in 200 ml of methylene chloride, dried over anhydrous magnesium sulfate and stripped under vacuum. The residue was distilled under vacuum and the product, b.p. 98°-106° C. at 0.15 mm, weighed 94 g and was 97% pure by GLPC. It was characterized by IR and NMR.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04723986uspto-grants-1988_02