반응 #216539

ord-6261e6ad67cc4ea18f5f2c8f819a22af

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated under argon for 24 hrs
  2. 2
    온도The reaction mixture was cooled
  3. 3
    세척washed with saturated aqueous sodium bicarbonate
  4. 4
    건조The organic layer was dried over magnesium sulfate
  5. 5
    여과filtered
  6. 6
    기타evaporated to dryness under vacuum
  7. 7
    기타to give an off-white solid
  8. 8
    기타The crude product was recrystallized from methanol

실험 절차

Dodecanoyl chloride (2.95 ml, 12.8 mmol) was added to a suspension of 2,4,6-triiodophenol (6.0 g, 12.7 mmol) in refluxing acetonitrile (50 ml) and the mixture was heated under argon for 24 hrs. The reaction mixture was cooled and washed with saturated aqueous sodium bicarbonate. The organic layer was dried over magnesium sulfate, filtered, and evaporated to dryness under vacuum to give an off-white solid. The crude product was recrystallized from methanol to give 6.9 g (83%) of the desired ester, mp 68°-69° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05468466uspto-grants-1995_11