반응 #991363

반응 방정식

O-methylcaprolactam

HCl

thiocarbohydrazide

→

4-amino-5-(5-aminopentyl)-4H-1,2,4-triazole-3-thiol hydrochloride

수율 56.4%

용매

methanol

반응 조건

후처리

1. 1
   온도After heating
2. 2
   온도at reflux for 2 hours
3. 3
   기타The solid product is recrystallized twice from methanol/ethyl acetate

실험 절차

To 200 ml of methanol is added 3.6 g (0.1 mole) of gaseous HCl followed by 12.7 g (0.1 mole) of O-methylcaprolactam and then 10.6 g (0.1 mole) of thiocarbohydrazide. After heating at reflux for 2 hours, the mixture is allowed to cool to room temperature and is refrigerated. The solid product is recrystallized twice from methanol/ethyl acetate, affording 13.4 g of 4-amino-5-(5-aminopentyl)-4H-1,2,4-triazole-3-thiol hydrochloride. m.p. 192°-194° C.

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