Реакция #487562

Уравнение реакции

potassium carbonate

lead tetraacetate

5-bromo-2-ethylphenylboronic acid

→

5-bromo-2-ethylphenyllead triacetate

Выход 67.2%

Условия реакции

Обработка

1. 1
   Другоеthoroughly flushed with nitrogen
2. 2
   workup.ADDITIONis added anhydrous chloroform (42 ml)
3. 3
   Температураthe suspension is heated at this temperature for 5 hours
4. 4
   Температураto cool to room temperature
5. 5
   Температураby further cooling to 0° C.
6. 6
   Фильтрацияfiltration
7. 7
   КонцентрированиеThe filtrate is concentrated to half its volume
8. 8
   workup.ADDITIONfollowed by the addition of hexanes
9. 9
   Другоеprecipitation
10. 10
    Другоеthe solvent decanted
11. 11
    Промывкаthe solid washed with hexanes

Методика

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.

Источник