反応 #54926

反応方程式

benzimidic acid 2-methylhydrazide hydrochloride

o-toluic acid chloride

→

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

収率 76.0%

溶媒

diethyl ether

反応条件

後処理

1. 1
   workup.ADDITIONA mixture of 0.56 g
2. 2
   温度After cooling
3. 3
   その他the hydrochloride of the triazole is collected
4. 4
   ろ過on filter
5. 5
   抽出The free base is extracted with diethyl ether
6. 6
   乾燥the organic phase, after drying over sodium sulfate
7. 7
   その他is evaporated
8. 8
   workup.DISTILLATIONThe crude compound is purified by distillation at 160° C./0.1 mm Hg

実験手順

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%.

出典