Dimethyl Sulfide → HCID 15132167, compound

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Reaction Steps

Me2S in THF (13.25 ml) was added dropwise to the product obtained in Example III (2.55 g, 0.008 mol) dissolved in 30 ml of THF with stirring and cooling in an ice bath. The ice bath was removed and the mixture was heated to reflux for 3.5 hours. The mixture was left to stand at room temperature overnight. Ethanolic HCl was added dropwise to the mixture with cooling (ice bath) and stirring until a pH of 1.5 was reached. The mixture was heated to reflux for one hour and then the solvent was removed. The residue was stirred with ether and 1N NaOH. The dried ether solution was evaporated in vacuo. The residue was crystallized from isopropyl ether, m.p. 98°-100° C. [α]26D +67.3 (DMF, c=1).

Provenance & Evidence