Hydrochloric Acid → HCID 20148320, compound

Participants

Reaction Conditions

Reaction Steps

2-Amino-5-[difluoro(isopropylthio)methyl]-1,3,4-thiadiazole (190 g) was dissolved in a mixture of acetic acid (880 ml) and concentrated hydrochloric acid (216.5 ml) at 60° C. A solution of sodium nitrite (171.3 g) in water (300 ml) was then added dropwise over 30 minutes at 65°-70° C. The mixture was stirred at 65° C. for 15 minutes and then allowed to cool. It was then poured onto water (3 L) and extracted with ether, the combined extracts being washed with water, dried (MgSO4) and evaporated to give an orange liquid, which was distilled under vacuum to give 150 g of 2-chloro-5-[difluoro(isopropylthio)methyl]-1,3,4-thiadiazole, bp 75°-77° C. at 0.7 mmHg.

Provenance & Evidence