Sodium hydrosulfide → 4-Chloro-2-(1,1-dimethylethyl)-5-mercapto-3(2H)-pyridazinone

Participants

Reaction Conditions

Reaction Steps

To 560 ml of water were added 66.3 g of 2-tert.-butyl-4,5-dichloro-3(2H)-pyridazinone and 48.0 g of 70% sodium hydrosulfide. After stirring at 60° C. for 4 hours activated carbon was added thereto. The resulting mixture was allowed to cool and then filtered. Concentrated hydrochloric acid was added to the resulting filtrate until the pH thereof was lowered to 2 or less. The resulting solid was filtered off, washed with water, dried and then recrystallized from a mixed solvent of benzene and n-hexane to give the intended product as white needle-like crystals of m.p. 112°-113° C. (yield: 81.5%).

Provenance & Evidence