Dimethylformamide → HCID 20563052、化合物

HRID 2286707

反応式

HRID 2286707 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-cc9dfb450b1b4e0c89dd1652681c6a96
出典データセット
uspto-grants-1981_05
特許番号
US04267332

関連ノート

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