反応 #5380

ord-b2461ebc65244f8f8d1cf4f61ec82c12

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度by refluxing for 310 minutes
  2. 2
    抽出extracted from ethyl acetate
  3. 3
    その他to obtain an organic layer
  4. 4
    洗浄The organic layer was washed with water
  5. 5
    乾燥dried with mirabilite
  6. 6
    その他dried under reduced pressure
  7. 7
    その他to obtain a resultant
  8. 8
    その他The resultant was recrystallized from ethylacetate
  9. 9
    その他to obtain a crystal
  10. 10
    ろ過The crystal was filtered
  11. 11
    その他purified by silica gel column chromatography (eluent: toluene)
  12. 12
    その他recrystallized from acetone

実験手順

In a 30ml round-bottom flask, 0.47 g (1.48 m mole) of 2-(6-hydroxy-2-naphthyl)-5-butylbenzooxazole, 0.43 g (1.79 m mole) of octyl iodide, 0.12 g (1.82 m mole) of potassium hydroxide and 5 ml of butanol were placed, followed by refluxing for 310 minutes. The reaction mixture was poured into water, extracted from ethyl acetate to obtain an organic layer. The organic layer was washed with water dried with mirabilite and dried under reduced pressure to obtain a resultant. The resultant was recrystallized from ethylacetate to obtain a crystal. The crystal was filtered, purified by silica gel column chromatography (eluent: toluene) and recrystallized from acetone to obtain 0.36 g of 2-(6-octyloxy-2-naphthyl)-5-butylbenzooxazole (Yield: 56.6%). ##STR190##

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05244596uspto-grants-1993_09