Reacción #487557

ord-99e333eb388c4b31b9b81b7e8ce74091

Ecuación de reacción

CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].[Pb+4]
lead tetraacetate
CCc1ccc(-c2ccc(Cl)cc2)cc1B(O)O
4′-chloro-4-ethylbiphen-3-ylboronic acid
CC(=O)[O-].CC(=O)[O-].CC(=O)[O-].CCc1ccc(-c2ccc(Cl)cc2)c[c]1[Pb+3]
4′-chloro-4-ethylbiphen-3-yllead triacetate
Rendimiento 100.0%

Condiciones de reacción

Temperatura
40°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothoroughly flushed with nitrogen
  2. 2
    workup.ADDITIONis added anhydrous chloroform (6 ml)
  3. 3
    Temperaturathe suspension is heated at this temperature for 5 hours
  4. 4
    TemperaturaThe mixture is then cooled to room temperature
  5. 5
    Concentraciónconcentrated to a small volume
  6. 6
    Otrotriturated with hexanes
  7. 7
    Filtraciónfiltered

Procedimiento

To a mixture of lead tetraacetate (2.15 g, 4.85 mmol) and mercuric diacetate (0.15 g, 0.47 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (6 ml). This mixture is warmed to 40° C., and 4′-chloro-4-ethylbiphen-3-ylboronic acid (1.17 g, 4.50 mmol) is added in one portion and the suspension is heated at this temperature for 5 hours. The mixture is then cooled to room temperature, concentrated to a small volume and triturated with hexanes and filtered to yield crude 4′-chloro-4-ethylbiphen-3-yllead triacetate (2.70 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08741806B2uspto-grants-2014_06