반응 #5380

ord-b2461ebc65244f8f8d1cf4f61ec82c12

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도by refluxing for 310 minutes
  2. 2
    추출extracted from ethyl acetate
  3. 3
    기타to obtain an organic layer
  4. 4
    세척The organic layer was washed with water
  5. 5
    건조dried with mirabilite
  6. 6
    기타dried under reduced pressure
  7. 7
    기타to obtain a resultant
  8. 8
    기타The resultant was recrystallized from ethylacetate
  9. 9
    기타to obtain a crystal
  10. 10
    여과The crystal was filtered
  11. 11
    기타purified by silica gel column chromatography (eluent: toluene)
  12. 12
    기타recrystallized from acetone

실험 절차

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##

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05244596uspto-grants-1993_09