Reacción #1901911

ord-5a63ab5bb6204fe0aacb73c0310cd7a0

Reactivos

Ninguno

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroare placed under argon at 0° C
  2. 2
    Otrohas returned gradually to room temperature
  3. 3
    OtroThe solvents are evaporated off under reduced pressure
  4. 4
    Otrothe white solid obtained
  5. 5
    Lavadois washed with dichloromethane
  6. 6
    workup.ADDITIONThe filtrate is treated with 50 ml of saturated aqueous sodium sulfate solution
  7. 7
    Lavadowashed with 50 ml of saturated aqueous sodium chloride solution
  8. 8
    Secadodried over magnesium sulfate
  9. 9
    OtroAfter evaporation of the solvents under reduced pressure
  10. 10
    Otroa yellow oil is obtained (quantitative yield)

Procedimiento

35 g of 1,4-benzodioxane and 200 ml of anhydrous dimethylformamide are placed under argon at 0° C. 54.9 g of N-bromosuccinimide are then added in portions. After it has returned gradually to room temperature, the reaction mixture is stirred for 24 hours. The solvents are evaporated off under reduced pressure and the white solid obtained is washed with dichloromethane. The filtrate is treated with 50 ml of saturated aqueous sodium sulfate solution, washed with 50 ml of saturated aqueous sodium chloride solution and dried over magnesium sulfate. After evaporation of the solvents under reduced pressure, a yellow oil is obtained (quantitative yield).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06878665B2uspto-grants-2005_04