THE FRIEDEL-CRAFTS REACTION: ACETYLATION OF FERROCENE
Ferrocene was acetylated in acetic anhydride and phosphoric acid. It proceeded via a Friedel-Crafts reaction without the use of organic solvents or strong Lewis acid.
Operations and Observations
A mixture of ferrocene (1.5 g, 0.008 mol), acetic anhydride (5 mL) and phosphoric acid (1 mL 85%) was heated over a steam bath until all the ferrocene dissolved and the mixture darkened from orange to dark red. The mixture was then refluxed with a calcium chloride drying tube for ten minutes and left to cool for an hour taking on a dark almost black colour. The reaction mixture was then poured onto ice (60 mL) and stirred to form brown mixture with some greenish black precipitate. Aqueous sodium hydroxide (37.5 mL, 3M) was added to the mixture and solid sodium bicarbonate was added until the mixture was neutralised. The mixture was left to stand for an hour with stirring before the crude product was collected with vacuum......
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