반응 #54926

반응 방정식

benzimidic acid 2-methylhydrazide hydrochloride

o-toluic acid chloride

→

1-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazole

수율 76.0%

용매

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONA mixture of 0.56 g
2. 2
   온도After cooling
3. 3
   기타the hydrochloride of the triazole is collected
4. 4
   여과on filter
5. 5
   추출The free base is extracted with diethyl ether
6. 6
   건조the organic phase, after drying over sodium sulfate
7. 7
   기타is evaporated
8. 8
   workup.DISTILLATIONThe crude compound is purified by distillation at 160° C./0.1 mm Hg

실험 절차

A mixture of 0.56 g. of benzimidic acid 2-methylhydrazide hydrochloride and 3.8 g. of o-toluic acid chloride is heated under stirring at about 120° C. After cooling and addition of diethyl ether, the hydrochloride of the triazole is collected on filter and then suspended in a sodium bicarbonate aqueous solution. The free base is extracted with diethyl ether and the organic phase, after drying over sodium sulfate, is evaporated. The crude compound is purified by distillation at 160° C./0.1 mm Hg. Yield 76%.

출처