Reacción #46458

ord-c9bb23be4d014b61b2df65620189bc16

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe DMF was removed under vacuum, and 1M HCl
  2. 2
    workup.ADDITIONwas added until the residue
  3. 3
    ExtracciónThe mixture was extracted with ethyl acetate
  4. 4
    Secadothe combined organic phase was dried over magnesium sulfate
  5. 5
    Filtraciónfiltered
  6. 6
    Concentraciónconcentrated under reduced pressure

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07741326B2uspto-grants-2010_06