Reaktion #3014

Reaktionsgleichung

2,6-dimethoxy-4-methylphenylboronic acid

lead tetraacetate

→

2,6-dimethoxy-4-methylphenyllead triacetate

Ausbeute 90.0%

Lösungsmittel

chloroform

chloroform

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITis then left
2. 2
   Sonstigeto return to room temperature
3. 3
   workup.STIRRINGThe reaction mixture is stirred at room temperature for 18 hours
4. 4
   FiltrationThe solution is filtered over a bed of celite
5. 5
   Sonstigethe solvent is then evaporated to dryness in order

Vorschrift

45.4 g of lead tetraacetate and 3.2 g of mercuric acetate are suspended in 150 ml of anhydrous chloroform and the mixture is heated to 40° C. under an argon atmosphere. A solution of 20 g of 2,6-dimethoxy-4-methylphenylboronic acid (prepared above) in 100 ml of chloroform is added dropwise to the reaction mixture at 40° C. The reaction mixture is left for 75 minutes at 40° C. and is then left to return to room temperature while stirring well. The reaction mixture is stirred at room temperature for 18 hours and is then diluted with 800 ml of dichloromethane. The solution is filtered over a bed of celite and the solvent is then evaporated to dryness in order to obtain yellow crystals of 2,6-dimethoxy-4-methylphenyllead triacetate, M.p.=172° C., Yield: 90%.

Quelle