Pyridine → HCID 20358860, 화합물

HRID 2082953노트

반응식

HRID 2082953 반응식
[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

참가 물질

5

반응물 2

HCID 1049PyridineHCID 136388401HCID 136388401, 화합물

생성물 1

HCID 20358860HCID 20358860, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-779c632f39cd4b028b4369303e49c2e0
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04083843

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