Abstract: A simple, efficient one-flask procedure for the largescale preparation of 3- carbomethoxy-3-sulfolene from trimethylphosphonoacetate is described. The procedure incorporates a cheap and simple sulfide to sulfone oxidation using Oxone®. No chromatography or intermediate purification steps are involved and the product is isolated by crystallisation. Key words: 3-carbomethoxy-3-sulfolene, 2, 5-dihydroxy-1, 4-dithiane, ...