تفاعل #54926

ord-7bda1585673340e6b793222737cca3f5

معادلة التفاعل

CNNC(=N)c1ccccc1.Cl
benzimidic acid 2-methylhydrazide hydrochloride
Cc1ccccc1C(=O)Cl
o-toluic acid chloride
Cc1ccccc1-c1nc(-c2ccccc2)nn1C
1-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazole
المردود 76.0%

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONA mixture of 0.56 g
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    أخرىthe hydrochloride of the triazole is collected
  4. 4
    ترشيحon filter
  5. 5
    استخلاصThe free base is extracted with diethyl ether
  6. 6
    تجفيفthe organic phase, after drying over sodium sulfate
  7. 7
    أخرىis evaporated
  8. 8
    workup.DISTILLATIONThe crude compound is purified by distillation at 160° C./0.1 mm Hg

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151169uspto-grants-1979_04