反应 #5380

ord-b2461ebc65244f8f8d1cf4f61ec82c12

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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##

来源

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