p-Toluenesulfonic acid → HCID 18185253, compound

Participants

Reaction Steps

14.9 g (0.1 mol) of 5-methyl-2,3,4,5-tetrahydrobenzoxepin-5-ol, 300 ml of toluene and a spatula tip of para-toluenesulphonic acid are charged to a 1 litre reactor equipped with a Denan and Stark apparatus. The combined solution is brought to reflux for 2 hours, the water being removed as it is formed. The reaction mixture is then neutralized with a 5% aqueous sodium bicarbonate solution and the organic solution is washed with water. The organic phase is subsequently dried over anhydrous sodium sulphate and concentrated under reduced pressure. 16 g of the title compound are obtained, which compound is purified by distillation, B.p. (2.5 mm Hg)=80-90° C. 10 g of a colourless liquid are obtained.

Provenance & Evidence