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Aniline → N-cyano-N'-phenyl-4-pyridinecarboximidamide

HRID 1588548
ノート
印刷プレビュー

反応式

HRID 1588548 の反応式
[C:1]([N:3]=[C:4]([C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)OC(C)C)#[N:2].[NH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[CH:11][N:12]=[CH:13][CH:14]=1)=[N:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6115AnilineHCID 10012715Isopropyl N-cyano-4-pyridinecarboximidate

生成物 1

HCID 19734506N-cyano-N'-phenyl-4-pyridinecarboximidamide収率 54%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Isopropyl N-cyano-4-pyridinecarboximidate (0.50 g, 2.6 mmol) was dissolved in methanol (5 ml), and aniline (0.27 g, 2.9 mmol) dissolved in methanol (5 ml) was added. The mixture was stirred at room temperature for 20 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residual concentrate was subjected to chromatography on a silica gel column (WAKO GEL C-200, 40 g). Elution with chloroform-methanol (100:1) gave the object compound, which was further crystallized from methanol-diethyl ether to give N-cyano-N'-phenyl-4-pyridinecarboximidamide (0.32 g, 1.4 mmol, yield: 54%) as colorless needles.

後処理

  1. additionwas added
  2. concentrationthe reaction solution was concentrated under reduced pressure
  3. concentrationThe residual concentrate
  4. washElution with chloroform-methanol (100:1)
  5. customgave the object compound, which
  6. customwas further crystallized from methanol-diethyl ether

出典と根拠

ORDレコード
ord-4342e46d1d33497e8d2e0771669afde3
出典データセット
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05223508

反応ノート

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