Acetic Acid → HCID 14695085, compound

Participants

Reaction Conditions

Reaction Steps

In 50 ml of acetic acid, 1.9 g of 2-hexylthio-7-methoxy-6-nitro-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one and 0.1 g of sodium tungstate dihydrate were dissolved. The solution was warmed to 50° C., and 3.1 g of a 30% hydrogen peroxide solution was added dropwise, and thereafter the solution was stirred at 52° C. for 1 hour. The reaction mixture was poured into 500 ml of water, and the formed precipitate was collected by filtration. The precipitate was washed with a sodium hydrogen sulfite aqueous solution and water, and recrystallized from ethanol. Thus 1.5 g of 2-hexanesulfonyl-7-methoxy-6-nitro-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one as colorless prismatic crystals was obtained. m.p. 150°~152° C. Yield 71%.

Provenance & Evidence