تفاعل #1558052

معادلة التفاعل

potassium carbonate

lead tetraacetate

5-bromo-2-methylphenylboronic acid

→

5-bromo-2-methylphenyllead triacetate

المردود 78.9%

ظروف التفاعل

المعالجة

1. 1
   أخرىthoroughly flushed with nitrogen
2. 2
   workup.ADDITIONis added anhydrous chloroform (35 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
   workup.ADDITIONis added
7. 7
   ترشيحThe mixture is filtered
8. 8
   تركيزthe filtrate is concentrated to half its volume, and hexanes
9. 9
   workup.ADDITIONadded
10. 10
    أخرىprecipitation
11. 11
    أخرىthe solvent decanted
12. 12
    غسيلthe solid washed with hexanes

الإجراء التجريبي

To a mixture of lead tetraacetate (11.25 g, 25.40 mmol) and mercuric diacetate (0.40 g, 1.27 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (35 ml). This mixture is warmed to 40° C., and 5-bromo-2-methylphenylboronic acid (4.96 g, 23.10 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 powdered anhydrous potassium carbonate (1.61 g) is added with rapid stirring for 5 minutes. The mixture is filtered, the filtrate is concentrated to half its volume, and hexanes added to induce precipitation. This mixture is further concentrated, the solvent decanted, and the solid washed with hexanes to afford 5-bromo-2-methylphenyllead triacetate (10.10 g) as a sandy coloured solid.

المصدر