Reaktion #68756

Reaktionsgleichung

lead(IV)acetate

5-bromo-2-cyclopropylphenyl boronic acid

potassium carbonate

→

5-bromo-2-cyclopropylphenyl lead triacetate

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution is heated at this temperature for 5 hours
2. 2
   Temperaturis further cooled to 0° C.
3. 3
   FiltrationThe reaction mixture is then filtered
4. 4
   Waschen(washing with additional chloroform)
5. 5
   Einengenthe filtrate is concentrated to half its original volume
6. 6
   Sonstigethe crude product is precipitated with hexanes
7. 7
   EinengenFurther concentration
8. 8
   Filtrationfiltration

Vorschrift

To a solution of lead(IV)acetate (4.0 g, 0.0089 mol) and mercury(II)acetate (139 mg, 0.45 mmol) in chloroform (12 ml) at 50° C. is added 5-bromo-2-cyclopropylphenyl boronic acid (2.0 g, 0.0083 mol), and the solution is heated at this temperature for 5 hours. After cooling to room temperature the suspension is further cooled to 0° C. and anhydrous potassium carbonate (1.8 g) is added with rapid stirring for 2 minutes. The reaction mixture is then filtered (washing with additional chloroform), and the filtrate is concentrated to half its original volume and the crude product is precipitated with hexanes. Further concentration then filtration affords 5-bromo-2-cyclopropylphenyl lead triacetate as a beige solid.

Quelle