Hydroxyamine hydrochloride → HCID 178516735, Verbindung

HRID 129443

Reaktionsgleichung

Reaktionsgleichung von HRID 129443
[N:1]1[C:2]2[C:14](=O)[C:13]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:3]=2[NH:4][C:5](=[O:7])[CH:6]=1.Cl.[NH2:17][OH:18]>N1C=CC=CC=1>[OH:18][N:17]=[C:14]1[C:2]2[N:1]=[CH:6][C:5](=[O:7])[NH:4][C:3]=2[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:13]1=2

Komponenten

4

Edukt 2

HCID 443297Hydroxyamine hydrochlorideHCID 190359769H-Indeno[1,2-b]pyrazine-3,9(4H)-dione

Produkt 1

HCID 178516735HCID 178516735, VerbindungAusbeute 49 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 9H-indeno[1,2-b]pyrazine-3,9(4H)-dione (1.0 g, 5.0 mmol), pyridine (40 ml) and hydroxylamine hydrochloride (0.42 g, 6.0 mmol) was stirred at 80° C. for 18 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with water, acetic acid and water and dried. The crude material (0.81 g) was recrystallized from DMF to afford 0.52 g (49%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 7.49-7.62 (m, 2H), 7.88 (d, 1H), 7.95 (s, 1H), 8.36 (d, 1H), 12.5-13.2 (broad, 1H), 12.83 (s, 1H).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationthe precipitate was filtered off
  3. washwashed with water, acetic acid and water
  4. customdried
  5. customThe crude material (0.81 g) was recrystallized from DMF

Quellen und Nachweise

ORD-Eintrag
ord-b2ba53c1c31a49e8888e0bd501cee82c
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05468748

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