반응 #62967

ord-58fe152fc2844904a472c431c60d2ea8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture heated to reflux
  2. 2
    온도at reflux temperatures
  3. 3
    workup.ADDITIONis added
  4. 4
    온도the reaction medium is heated
  5. 5
    온도at reflux temperature for about 15 hours
  6. 6
    기타Ethanol is removed under vacuum from the cooled mixture
  7. 7
    여과filtered
  8. 8
    세척washed with water, and air
  9. 9
    기타dried
  10. 10
    기타The product then is recrystallized from 90/10 hexane/toluene, mp 74°-76° C.

실험 절차

To 400 ml ethanol is added 21.5 g of 4-hydroxy-4'-nitrobiphenyl, and the mixture heated to reflux. A solution of 7.1 g KOH in 30 ml of water is added dropwise at reflux temperatures. After complete addition, 18 g of 5-bromo-1-pentene is added and the reaction medium is heated at reflux temperature for about 15 hours. Ethanol is removed under vacuum from the cooled mixture, and the solid residue is slurried with water in a blender, filtered, washed with water, and air dried. The product then is recrystallized from 90/10 hexane/toluene, mp 74°-76° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04762912uspto-grants-1988_08