반응 #735376

반응 방정식

thiocarbohydrazide

hydroxyacetic acid

→

crystals

수율 47.9%

4-Amino-5-mercapto-4H-1,2,4-triazole-3-methanol

수율 47.9%

용매

water

반응 조건

후처리

1. 1
   온도were heated
2. 2
   온도The mixture is cooled to room temperature
3. 3
   온도It is then cooled for 24 hours at 11° C.

실험 절차

A mixture of 10.6 g (0.1 mole) of thiocarbohydrazide and 25.0 g (0.33 mole) of hydroxyacetic acid were heated and stirred at 130° C. for 20 minutes. The mixture is cooled to room temperature and diluted with 25 ml of water. It is then cooled for 24 hours at 11° C., yielding 7.0 g of crystals. The latter are recrystallized from chloroform/methanol, affording 4.5 g of solvated product. The product is dried in vacuo, affording 2.0 g of pale yellow crystals of 4-amino-5-mercapto-4H-1,2,4-triazole-3-methanol. m.p. 150.5°-151.5° C. When the reaction is repeated, using a longer heating time, (1 hour at 125° C.), and is followed by recrystallization from methanol/water, a higher yield of the same product is obtained (80% ).

출처