Reaktion #487562

Reaktionsgleichung

potassium carbonate

lead tetraacetate

5-bromo-2-ethylphenylboronic acid

→

5-bromo-2-ethylphenyllead triacetate

Ausbeute 67.2%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethoroughly flushed with nitrogen
2. 2
   workup.ADDITIONis added anhydrous chloroform (42 ml)
3. 3
   Temperaturthe suspension is heated at this temperature for 5 hours
4. 4
   Temperaturto cool to room temperature
5. 5
   Temperaturby further cooling to 0° C.
6. 6
   Filtrationfiltration
7. 7
   EinengenThe filtrate is concentrated to half its volume
8. 8
   workup.ADDITIONfollowed by the addition of hexanes
9. 9
   Sonstigeprecipitation
10. 10
    Sonstigethe solvent decanted
11. 11
    Waschenthe solid washed with hexanes

Vorschrift

To a mixture of lead tetraacetate (13.7 g, 31.00 mmol) and mercuric diacetate (0.47 g, 1.50 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (42 ml). This mixture is warmed to 40° C., and 5-bromo-2-ethylphenylboronic acid (6.50 g, 28.00 mmol) is added in one portion and the suspension is heated at this temperature for 5 hours. The mixture is then allowed to cool to room temperature, followed by further cooling to 0° C. then addition of powdered anhydrous potassium carbonate (3.22 g) with rapid stirring for 5 minutes then filtration. The filtrate is concentrated to half its volume, followed by the addition of hexanes to induce precipitation. This mixture is further concentrated, the solvent decanted, and the solid washed with hexanes to afford 5-bromo-2-ethylphenyllead triacetate (10.69 g) as a sandy coloured solid.

Quelle