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p-Toluidine → HCID 178424384、化合物

HRID 2304430
ノート
印刷プレビュー

反応式

HRID 2304430 の反応式
[C:1]1([CH3:14])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][N:8]=[C:9]([C:12]#[N:13])[C:10]#[N:11].NC1C=CC(C)=CC=1.C(#N)CC#N.O.[NH2:29][NH2:30]>>[NH2:11][C:10]1[C:9](=[N:8][NH:7][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[CH3:14])[C:12]([NH2:13])=[N:30][N:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 7813p-ToluidineHCID 8010MalononitrileHCID 24654Hydrazine hydrate (1:1)HCID 12450559Carbonylcyanide2methylphenylhydrazone

生成物 1

HCID 178424384HCID 178424384、化合物収率 40%

実験手順

This compound was prepared using 92 mg (0.5 mmol) of 2-(o-tolylhydrazono)-malononitrile, which was derived from 4-toluidine (107 μL, 1.0 mmol) and malononitrile (1.5 mmol) as described in Example 8, and hydrazine hydrate. Very little solid had formed after heating the reaction at 75° C. for 1 hr, however, analysis of the reaction solution by TLC indicated that no starting material remained. The solution was allowed to cool to room temperature and the solvent was evaporated. The residue was dissolved in ethyl acetate and then precipitated by the addition of hexanes. The resulting solid was isolated by filtration and dried to yield 43 mg (40%) of the title compound as a yellow solid.

後処理

  1. customThis compound was prepared
  2. customVery little solid had formed
  3. temperatureafter heating
  4. customthe reaction at 75° C. for 1 hr
  5. customthe solvent was evaporated
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. customprecipitated by the addition of hexanes
  8. customThe resulting solid was isolated by filtration
  9. customdried

出典と根拠

ORDレコード
ord-19019dc59fb1454aa352515c0968e36d
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06436915B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート