p-Toluenesulfonic acid → HCID 21904108, compound

Participants

Reaction Steps

Using a 15 cm Wiedmer distillation apparatus, a solution of 50 mmol of 3-methyl acetophenone in 15.02 g (150 mmol) of isopropenyl acetate was heated at 95° in the presence of 75 mg of para-toluene sulphonic acid. At a stabilised conversion (50–70% by GC, after 8 h at 95°), the mixture was cooled and 300 mg of trioctylamine were added. After extraction by means of ether, and usual workup, the product was distilled on a bulb-to-bulb apparatus and purified by preparative GC using a 1.2 m×6 mm column loaded with 10% SE-30 on Supelcoport® 80–100 mesh, vector gas: helium at 30 ml/min. The product was obtained in 60% yield

Provenance & Evidence