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p-Toluidine → HCID 178424384、化合物

HRID 254960
ノート
印刷プレビュー

反応式

HRID 254960 の反応式
C1(C)C=CC=CC=1[NH:7][N:8]=[C:9]([C:12]#[N:13])[C:10]#[N:11].N[C:16]1[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=1.C(#N)CC#N.O.[NH2:29][NH2:30]>>[C:19]1([CH3:22])[CH:20]=[CH:21][CH:16]=[CH:17][C:18]=1[NH:7][N:8]=[C:9]1[C:10]([NH2:11])=[N:30][N:29]=[C:12]1[NH2:13]
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

実験手順

4-(o-tolylhydrazono)-4H-pyrazole-3,5-diamine 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), 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 ambient 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 compound as a yellow solid.

後処理

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

出典と根拠

ORDレコード
ord-6a70b60cf70c4fa887085f6d31139810
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07875728B2

反応ノート

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