Dimethylformamide → HCID 20563052、化合物

HRID 613982

反応式

HRID 613982 の反応式
N[C:2]1[O:3][C:4]2[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=2[C:6](=[O:10])[C:7]=1C=O.[C:15]([C:17]#[CH:18])#[N:16].[CH3:19][N:20](C)C=O>>[C:15]([C:17]1[CH:19]=[N:20][C:7]2[C:6](=[O:10])[C:5]3[C:4]([O:3][C:2]=2[CH:18]=1)=[CH:14][CH:13]=[CH:12][CH:11]=3)#[N:16]

参加物

4

反応条件

温度
140 °C

実験手順

To 70 ml of dimethylformamide was added 2.2 g of 2-amino-4-oxo-4H-1-benzopyran-3-carboxaldehyde, followed by the addition of 2.5 g of cyanoacetylene. The mixture was heated under stirring at 140° C. for 15 hours and the solvent was then distilled off under reduced pressure. The residue was chromatographed on silica gel and eluted with chloroform and recrystallized from acetonitrile to give 0.83 g of 3-cyano-1-azaxanthone as crystals, m.p. 220°-226° C.

後処理

  1. temperatureThe mixture was heated
  2. distillationthe solvent was then distilled off under reduced pressure
  3. customThe residue was chromatographed on silica gel
  4. washeluted with chloroform
  5. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-53216e11e18842ada0acdfc09a4e3e2b
出典データセット
uspto-grants-1979_03
特許番号
US04143042

関連ノート

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