Methanesulfenylchloride → HCID 54725953, compound

Participants

Reaction Conditions

Reaction Steps

Methanesulfenyl chloride (21.6 g., 0.261 mol) dissolved in methylene chloride (100 ml.) was added to a rapidly stirred slurry of the monosodium salt of 4-hydroxy-6-methyl-2-pyrone (38.6 g., 0.261 mol) in methylene chloride (500 ml.) over a period of 35 minutes. The reaction temperature was maintained at 25°C. with cooling during the addition; then stirring was continued at ambient temperature for 4 hours. The methylene chloride was removed by distillation in vacuo and the residue triturated with water (200 ml.) to remove the by-product sodium chloride. The crude product was removed by filtration, 26.0 g., m. 127°-134°C., 58 percent yield; after recrystallization from 2-propanol, 17.2 g., m. 139°-140.5°C., 38 percent yield

Provenance & Evidence