반응 #487562

반응 방정식

potassium carbonate

lead tetraacetate

5-bromo-2-ethylphenylboronic acid

→

5-bromo-2-ethylphenyllead triacetate

수율 67.2%

반응 조건

후처리

1. 1
   기타thoroughly flushed with nitrogen
2. 2
   workup.ADDITIONis added anhydrous chloroform (42 ml)
3. 3
   온도the suspension is heated at this temperature for 5 hours
4. 4
   온도to cool to room temperature
5. 5
   온도by further cooling to 0° C.
6. 6
   여과filtration
7. 7
   농축The filtrate is concentrated to half its volume
8. 8
   workup.ADDITIONfollowed by the addition of hexanes
9. 9
   기타precipitation
10. 10
    기타the solvent decanted
11. 11
    세척the solid washed with hexanes

실험 절차

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.

출처