تفاعل #214884

ord-7c3c9875c0534acdaf565b093f156b5a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
260°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONis added
  2. 2
    درجة الحرارةthe resulting solution is heated
  3. 3
    درجة الحرارةat reflux for 30 minutes
  4. 4
    درجة الحرارةAfter cooling
  5. 5
    ترشيحthe intermediate acylamidrazone is collected by filtration
  6. 6
    درجة الحرارةafter which the reaction is cooled to room temperature
  7. 7
    أخرىUpon recrystallization from acetonitrile-water

الإجراء التجريبي

Sodium (0.4 grams) is added to pyridine-4-carbonitrile (8.3 grams, 0.08 mole) in methanol, and the solution is allowed to stand 30 minutes at room temperature. A suspension of pyrazine carboxylic acid hydrazide (9.6 grams, 0.07 mole) in methanol (160 ml.) is added, and the resulting solution is heated at reflux for 30 minutes. After cooling, the intermediate acylamidrazone is collected by filtration. The acyclic intermediate is then heated at 260° C. for 15 minutes, after which the reaction is cooled to room temperature. Upon recrystallization from acetonitrile-water, 3-pyrazinyl-5-(4-pyridyl)-1,2,4-triazole is obtained, m.p. 251°-252.5° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04256887uspto-grants-1981_03