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Dimethylformamide → HCID 20563001、化合物

HRID 1155192
ノート
印刷プレビュー

反応式

HRID 1155192 の反応式
N[C:2]1[O:3][C:4]2[CH:14]=[CH:13][C:12]([CH2:15][CH3:16])=[CH:11][C:5]=2[C:6](=[O:10])[C:7]=1C=O.[C:17]([CH2:19][C:20](Cl)=O)#[N:18].C[N:24]([CH3:27])C=O>>[CH2:15]([C:12]1[CH:11]=[C:5]2[C:4]([O:3][C:2]3[CH:20]=[C:19]([C:27]#[N:24])[CH:17]=[N:18][C:7]=3[C:6]2=[O:10])=[CH:14][CH:13]=1)[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 110515942-Cyanoacetyl chlorideHCID 126892482-Amino-6-ethyl-4-oxo-4H-1-benzopyran-3-carbaldehyde

生成物 1

HCID 20563001HCID 20563001、化合物

実験手順

In 40 ml of dimethylformamide was dissolved 1.82 g of 2-amino-6-ethyl-4-oxo-4H-1-benzopyran-3-carboxaldehyde, followed by the addition of 3.5 g of cyanoacetyl chloride. The mixture was reacted at 60° C. for 3 hours, with constant stirring. The solvent was then distilled off under reduced pressure and the residue was chromatographed on silica gel. The desired product was recovered from the chloroform eluate and recrystallized from acetonitrile. By the above procedure was obtained 1.03 g of 7-ethyl-3-cyano-1-azaxanthone, m.p. 183°-185° C.

後処理

  • customThe mixture was reacted at 60° C. for 3 hours, with constant stirring
  • distillationThe solvent was then distilled off under reduced pressure
  • customthe residue was chromatographed on silica gel
  • customThe desired product was recovered from the chloroform eluate
  • customrecrystallized from acetonitrile
  • 出典と根拠

    ORDレコード
    ord-e88ccafbaee546479f9f159f64d06ef3
    出典データセット
    uspto-grants-1981_11
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04299963

    反応ノート

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