Hydrochloric Acid → 1H-1,2,4-triazol-5-ylthiourea

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Reaction Steps

N-(1,2,4-triazol-5-yl)-N'-benzoylthiourea (26.0 g, 0.105 mole), from Example 6, was added at once to approximately 100ml of a 10% sodium hydroxide solution which had been preheated to boiling, and the resultant mixture was refluxed for 45 minutes. The solution was then cooled and acidified to approximately pH 3 with the addition of concentrated hydrochloric acid to provide a white solid precipitate. The solid was filtered, washed with water and dried for about 16 hours in a vacuum oven at approximately 100° C. The resultant off-white solid was stirred with about 150 ml of diethyl ether and filtered, and this procedure was repeated. The solid thus obtained was dried in a vacuum oven at about 50° C. to yield 10.4 g (69%) of N-(1,2,4-triazol-5-yl)thiourea as an off-white solid. The structural assignment was confirmed by nuclear magnetic resonance spectral analysis.

Provenance & Evidence