p-Toluenesulfonic acid → HCID 18976425, compound

Participants

Reaction Steps

A solution of 1.10 gm (3.19 mmol) of 2-[3-(3-bromo-2,5-dimethoxyphenyl)propyl]-1,3-dioxane and 300 mg p-toluene sulphonic acid in 10 ml absolute ethanol was refluxed for 48 hours at which time tlc analysis (silica gel, 1:4 ethyl acetate:hexane) indicated the absence of the dioxane. The solvent was removed in vacuo and the residue was partitioned between ether and 5% sodium carbonate. The ether extract was washed with brine, dried with Na2SO4, filtered and the solvent was removed in vacuo. The residue was kugelrohr distilled at 0.005 mm Hg to give 0.85 gm (99%) of a colorless oil, bp 95° C. (air bath temperature), homogeneous by tlc (ibid), Rf 0.74.

Provenance & Evidence