Hydrochloric Acid → HCID 15030536, compound

Participants

Reaction Steps

36.0 g (0.227 mol) of 2-acetyl-3-keto-4-methyl-4,5-dihydrothiophene are initially introduced into 260 ml of methylene chloride 21.9 ml of sulphuryl chloride in 260 ml of methylene chloride are then added dropwise at 0° C. While the sulphuryl chloride/methylene chloride mixture is added dropwise, a stream of nitrogen is passed into the solution to expel the HCl gas which is formed. When the addition is complete, stirring is continued for 30 minutes at 10°-15° C. The mixture is then introduced into 600 ml of water, and the organic phase is extracted with a 5% strength NaHCO3 solution, dried and concentrated in vacuo.

Provenance & Evidence