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Aniline → HCID 9816404, Verbindung

HRID 1153731
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1153731
[N:1]1[C:10]2[C:9](=[O:11])[CH:8]=[CH:7][C:6](=[O:12])[C:5]=2[N:4]=[CH:3][CH:2]=1.[NH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[NH:13]([C:8]1[C:9](=[O:11])[C:10]2[N:1]=[CH:2][CH:3]=[N:4][C:5]=2[C:6](=[O:12])[CH:7]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
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Komponenten

4

Edukt 2

HCID 6115AnilineHCID 113556455,8-Quinoxalinedione

Produkt 1

HCID 9816404HCID 9816404, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Approximately 2 g. of 5,8-quinoxalinedione were dissolved in 200 ml. of 2B ethanol. Aniline (1.2 g.) was added and the reaction was stirred overnight at room temperature. The reaction was evaporated, water was added, and the mixture was extracted several times with methylene chloride. The combined extracts were dried over sodium sulfate and evaporated to dryness. The residue was chromatographed over a silica gel column, eluting with ethyl acetate. The desired fractions were combined and evaporated. The material was crystallized from ethyl acetate to give 50 mg. of the title product as a red powder, m.p. about 203°-205° C.

Aufarbeitung

  1. customThe reaction was evaporated
  2. additionwater was added
  3. extractionthe mixture was extracted several times with methylene chloride
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. customevaporated to dryness
  6. customThe residue was chromatographed over a silica gel column
  7. washeluting with ethyl acetate
  8. customevaporated
  9. customThe material was crystallized from ethyl acetate
  10. customto give 50 mg

Quellen und Nachweise

ORD-Eintrag
ord-fbcec31f3cfc4447831a40bac5b73036
Quelldatensatz
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04486432

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