Dimethylformamide → HCID 20563052, 화합물

HRID 127354

반응식

HRID 127354 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

HCID 20563052HCID 20563052, 화합물

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1024b56898ab4dc3a52291c2bd63f8af
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255576

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