Dimethylformamide → HCID 20563052、化合物

HRID 127354

反応式

HRID 127354 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

反応物 3

HCID 6228DimethylformamideHCID 140552-PropynenitrileHCID 7359282-Amino-3-formylchromone

生成物 1

HCID 20563052HCID 20563052、化合物

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-1024b56898ab4dc3a52291c2bd63f8af
出典データセット
uspto-grants-1981_03
特許番号
US04255576

関連ノート

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