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A 34.9 g portion of selenium dioxide was dissolved in a mixture of 85 ml of dioxane and 10 ml of water with stirring and heating to 55°-60° C. A 40 g portion of -acetyl-3-methylthiophene was added and the mixture was refluxed for 6 hours, then cooled, diluted with dioxane, filtered and evaporated to dryness. The residue was dissolved in ether and the crystals which formed collected, giving 12.03 g of 3-methyl-α-oxo-2-thiopheneacetaldehyde.

1. temperatureheating to 55°-60° C
2. temperaturethe mixture was refluxed for 6 hours
3. temperaturecooled
4. filtrationfiltered
5. customevaporated to dryness
6. dissolutionThe residue was dissolved in ether
7. customthe crystals which formed
8. customcollected