Reacción #2447208

ord-2498e969c9004950a573074878c50c3d

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaat reflux for 16 h
  3. 3
    Temperaturacooled
  4. 4
    Concentraciónconcentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in EtOAc
  6. 6
    Lavadowashed with water, brine
  7. 7
    Secadodried (Na2SO4)
  8. 8
    Filtraciónfiltered
  9. 9
    Concentraciónconcentrated

Procedimiento

A mixture of 2-hydroxy-3,5-diiodobenzoic acid (3.9 g, 10.0 mmol) potassium carbonate (4.15 g, 30.0 mmol) and dimethyl sulfate (2.77 g, 22.0 mmol) in acetone (33 ml) was heated at reflux for 16 h, cooled and concentrated. The residue was dissolved in EtOAc and washed with water, brine, dried (Na2SO4), filtered and concentrated to give an off-white solid (4.2 g, quantitative yield).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08685991B2uspto-grants-2014_04