Pyridine → HCID 20358860、化合物

HRID 2082953ノート

反応式

HRID 2082953 の反応式
[N:1]([C:12]1[NH:13][C:14]([C:19]#[N:20])=[C:15]([C:17]#[N:18])[N:16]=1)=[N:2][C:3]1[NH:4][C:5]([C:10]#[N:11])=[C:6]([C:8]#[N:9])[N:7]=1.N1C=CC=CC=1>[Zn].C(O)(=O)C>[NH:2]([C:3]1[NH:7][C:6]([C:8]#[N:9])=[C:5]([C:10]#[N:11])[N:4]=1)[NH:1][C:12]1[NH:13][C:14]([C:19]#[N:20])=[C:15]([C:17]#[N:18])[N:16]=1

参加物

5

反応物 2

HCID 1049PyridineHCID 136388401HCID 136388401、化合物

生成物 1

HCID 20358860HCID 20358860、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

2.65 g of 2,2'-azobis(4,5-imidazoledicarbonitrile) was placed in a flask with 65 ml of pyridine and 25 ml of galcial acetic acid. The slurry was then purged and deoxygenated thoroughly with a stream of nitrogen. Then 3 equivalents (1.95 g) of zinc dust was added. An immediate green/black solution was formed characteristic of a radical anion species. This slowly faded to a pale green as the last of the intermediate reacted. The mixture was filtered under nitrogen to remove excess zinc salts. This gave a pale yellow solution of 2,2'-hydrazobis(4,5-imidazoledicarbonitrile). Exposure of an aliquot to the air caused immediate air oxidation back to the bright yellow azo compound which precipitated as the bis pyridinium salt.

後処理

  1. customThe slurry was then purged
  2. customdeoxygenated thoroughly with a stream of nitrogen
  3. customAn immediate green/black solution was formed characteristic of a radical anion species
  4. customreacted
  5. filtrationThe mixture was filtered under nitrogen
  6. customto remove excess zinc salts

出典と根拠

ORDレコード
ord-779c632f39cd4b028b4369303e49c2e0
出典データセット
uspto-grants-1978_04
特許番号
US04083843

反応ノート

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