반응 #433420

ord-21d125186760420e8eb498b177e62f40

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도at reflux for 24 hr
  3. 3
    여과The mixture was filtered
  4. 4
    농축the filtrate was concentrated under reduced pressure
  5. 5
    기타to give an oil which
  6. 6
    기타gradually crystallized to a semi-solid
  7. 7
    기타The solid was recrystallized from ethyl ether-petroleum ether (30°-60°)

실험 절차

A mixture of 50 g (0.238 mole of ethyl homovanillate (98% Aldrich), 75 g (0.476 mole) of 1-bromo-3-chloropropane and 98.7 g (0.71 mole) of anhydrous potassium carbonate in 1 L of acetone was heated at reflux for 24 hr. The mixture was filtered and the filtrate was concentrated under reduced pressure to give an oil which gradually crystallized to a semi-solid. The solid was recrystallized from ethyl ether-petroleum ether (30°-60°) to yield 44.4 g (65%) of title compound a white solid, mp 36°-38° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05061720uspto-grants-1991_10