Reacción #68756

ord-7a0a3d5313034f89b09bb452f512b217

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe solution is heated at this temperature for 5 hours
  2. 2
    Temperaturais further cooled to 0° C.
  3. 3
    FiltraciónThe reaction mixture is then filtered
  4. 4
    Lavado(washing with additional chloroform)
  5. 5
    Concentraciónthe filtrate is concentrated to half its original volume
  6. 6
    Otrothe crude product is precipitated with hexanes
  7. 7
    ConcentraciónFurther concentration
  8. 8
    Filtraciónfiltration

Procedimiento

To a solution of lead(IV)acetate (4.0 g, 0.0089 mol) and mercury(II)acetate (139 mg, 0.45 mmol) in chloroform (12 ml) at 50° C. is added 5-bromo-2-cyclopropylphenyl boronic acid (2.0 g, 0.0083 mol), and the solution is heated at this temperature for 5 hours. After cooling to room temperature the suspension is further cooled to 0° C. and anhydrous potassium carbonate (1.8 g) is added with rapid stirring for 2 minutes. The reaction mixture is then filtered (washing with additional chloroform), and the filtrate is concentrated to half its original volume and the crude product is precipitated with hexanes. Further concentration then filtration affords 5-bromo-2-cyclopropylphenyl lead triacetate as a beige solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08530388B2uspto-grants-2013_09