Reacción #460743

ord-d55515ea6c4e476f9ef7d313838cc901

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.WAITleft
  2. 2
    Otroto react for 1 hour
  3. 3
    workup.ADDITIONIt was then poured on to ice
  4. 4
    Extracciónextracted with ether
  5. 5
    LavadoWashing with NaHCO3 solution and water
  6. 6
    Otrodrying
  7. 7
    Otroevaporation

Procedimiento

8.55 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodioxepine (see Example 10) were dissolved in 70 ml of methylene chloride (CH2Cl2) and treated at 0° C. under an Argon atmosphere with a solution of 8.0 of Br2 in 30 ml of CH2Cl2. The mixture was warmed to room temperature and left to react for 1 hour. It was then poured on to ice and extracted with ether. Washing with NaHCO3 solution and water, drying and evaporation yielded 13.35 of of 7-bromo-3,4-dihydro-3,3-dimethyl-2H-1,5-benzodioxepine as a colorless oil which was 94.5% pure and which contained 4.7% of starting material; it was processed in the crude state.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05164387uspto-grants-1992_11