Reacción #599764

ord-2660a104f465464fa90006c262d38d39

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONChloroform (20 ml) is added
  3. 3
    TemperaturaAfter further heating at 50° C. for 3 hours the reaction mixture
  4. 4
    Temperaturais cooled to 0° C.
  5. 5
    Filtraciónbefore filtering
  6. 6
    Otroevaporation of the crude solution under reduced pressure
  7. 7
    OtroThe crude product is then azeotroped with diethyl ether

Procedimiento

Lead tetraacetate (5.7 g, 0.013 mol) and mercury (II) acetate (0.2 g, 0.0006 mol) are stirred together and thoroughly flushed with nitrogen. Chloroform (20 ml) is added and the dark orange solution heated to 50° C., followed by the addition of 4-benzyloxy-2,6-dimethylphenyl boronic acid (3 g, 0.012 mol) in one portion. After further heating at 50° C. for 3 hours the reaction mixture is cooled to 0° C. and potassium carbonate added (1.9 g, 0.02 mol). The suspension is stirred for just 5 minutes before filtering and evaporation of the crude solution under reduced pressure. The crude product is then azeotroped with diethyl ether to afford 4-benzyloxy-2,6-dimethylphenyl lead triacetate as a pale solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09102642B2uspto-grants-2015_08