Hydrochloric Acid → HCID 14324507, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 600 g of N,N-dibutyl-4-chloro-3-nitrobenzenesulfonamide, 220 g of 5-methyl-3-hydroxyisoxazole, 300 g of sodium hydrogen carbonate and 1.5 liter of dimethylsulfoxide was reacted at 80° C. for 6 hours. The reaction mixture was cooled to 40° C., 1.2 liter of methanol was added thereto, and then 400 ml of concentrated hydrochloric acid was added thereto at 25° C. After stirring for 30 minutes, 800 ml of water was added thereto. The crystals thus deposited were collected by filtration, washed with water, recrystallized from methanol and dried. Yield: 613 g (86.6%). Melting point: 84° to 86° C.

Provenance & Evidence