تفاعل #487562

معادلة التفاعل

potassium carbonate

lead tetraacetate

5-bromo-2-ethylphenylboronic acid

→

5-bromo-2-ethylphenyllead triacetate

المردود 67.2%

ظروف التفاعل

المعالجة

1. 1
   أخرىthoroughly flushed with nitrogen
2. 2
   workup.ADDITIONis added anhydrous chloroform (42 ml)
3. 3
   درجة الحرارةthe suspension is heated at this temperature for 5 hours
4. 4
   درجة الحرارةto cool to room temperature
5. 5
   درجة الحرارةby further cooling to 0° C.
6. 6
   ترشيحfiltration
7. 7
   تركيزThe filtrate is concentrated to half its volume
8. 8
   workup.ADDITIONfollowed by the addition of hexanes
9. 9
   أخرىprecipitation
10. 10
    أخرىthe solvent decanted
11. 11
    غسيلthe solid washed with hexanes

الإجراء التجريبي

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.

المصدر