Chloral Hydrate → HCID 57046400, compound

Participants

Reaction Steps

In 20 ml of methanol were dissolved 0.99 g (6 mmole) of chloral hydrate and 0.93 g (5 mmole) of p-toluenesulfonylhydrazine, and the mixture was stirred at room temperature for 30 minutes to form trichloroacetaldehyde-p-toluenesulfonylhydrazone. Then, to the reaction mixture was added under room temperature 15 ml of a 30% hydrated methanol solution containing 1.7 g (25 mmole) of ammonium sulfide for 10 minutes. Thereafter, the reaction was continued for further 2 hours while maintaining the pH of the reaction system at 10.4 by using 28% aqueous ammonia, a 30% aqueous potassium hydroxide solution, etc. The analysis after completion of the reaction was carried out in the same manner as in Example 1. The yield of the 5-mercapto-1,2,3-thiadiazole salt referred to the starting p-toluenesulfonylhydrazine was 22%.

Provenance & Evidence