4-Cyanopyridine → HCID 178419986、化合物

HRID 263122

反応式

HRID 263122 の反応式
[Na].[N:2]1[CH:7]=[CH:6][C:5]([C:8]#[N:9])=[CH:4][CH:3]=1.[N:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:16]([NH:18][NH2:19])=O>CO>[N:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:16]1[N:9]=[C:8]([C:5]2[CH:6]=[CH:7][N:2]=[CH:3][CH:4]=2)[NH:19][N:18]=1

参加物

5

反応物 3

HCID 75064-CyanopyridineHCID 258796Pyrazine-2-Carboxylic Acid HydrazideHCID 5360545Sodium

生成物 1

HCID 178419986HCID 178419986、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
260 °C

実験手順

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.

後処理

  1. additionis added
  2. temperaturethe resulting solution is heated
  3. temperatureat reflux for 30 minutes
  4. temperatureAfter cooling
  5. filtrationthe intermediate acylamidrazone is collected by filtration
  6. temperatureafter which the reaction is cooled to room temperature
  7. customUpon recrystallization from acetonitrile-water

出典と根拠

ORDレコード
ord-2dd9c049b902440eb6c979fbf9c98166
出典データセット
uspto-grants-1979_05
特許番号
US04156085

関連ノート

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