Sulfuric Acid → Dibenzoylmethane

Participants

Reaction Conditions

Reaction Steps

Acetophenone (30 grams; 0.25 mol), methylbenzoate (130 grams, 1.0 mol), sodium methoxide (17.3 grams; 0.32 mol) and xylene (350 ml) were placed into a four necked round bottom one liter flask, equipped with stirrer, nitrogen addition adapter, thermometer and Oldershaw column connected with a distillation head and a trap. The solution was heated under a blanket of nitrogen to a temperature of about 130° C. At about 130° C., the mixture of xylene and methanol begins to come off the reaction mixture. Upon cooling the reaction mixture is acidified by adding sulfuric acid (21 ml) in water (100 ml). Once the material goes into solution it is transferred to a separatory funnel and the aqueous layer is removed. The xylene layer is washed with water (100 ml of a 10% solution). Then it is stirred at 120° C. and 15 mm Hg. The yield of dibenzoyl methane was 94 weight percent having a purity of 97%.

Provenance & Evidence