반응 #46458

ord-c9bb23be4d014b61b2df65620189bc16

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The DMF was removed under vacuum, and 1M HCl
  2. 2
    workup.ADDITIONwas added until the residue
  3. 3
    추출The mixture was extracted with ethyl acetate
  4. 4
    건조the combined organic phase was dried over magnesium sulfate
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure

실험 절차

2-Bromo-4-methyl-6-iodophenol (7.82 gm, 25 mmol) and cinnamyl bromide (4.93 g, 25 mmol) were added to DMF (20 ml). Diisopropylethylamine (5.3 ml, 30.4 mmol) was added and the mixture heated to 60° C. for 15 minutes and then allowed stir for 16 hours at room temperature. The DMF was removed under vacuum, and 1M HCl was added until the residue was acidic. The mixture was extracted with ethyl acetate, and the combined organic phase was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give 1-bromo-3-iodo-5-methyl-2-(3-phenylallyloxy)-benzene (10.86 g, 100% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741326B2uspto-grants-2010_06