HCID 22097096, Verbindung → HCID 22097212, Verbindung

HRID 1457558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1457558
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-])=O)[N:8]([CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[C:7](=[O:21])[C:6](=[O:22])[NH:5]2>O1CCCC1.CO.CN(C)C=O.[Pd]>[NH2:12][C:11]1[CH:10]=[C:9]2[C:4]([NH:5][C:6](=[O:22])[C:7](=[O:21])[N:8]2[CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:3][CH:2]=1

Komponenten

4

Edukt 1

HCID 22097096HCID 22097096, Verbindung

Produkt 1

HCID 22097212HCID 22097212, VerbindungAusbeute 80,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 86634690HCID 86634690, VerbindungLösungsmittel

Versuchsvorschrift

28.9 g (89 mmol) of 6-chloro-1-cyclohexyl-7-nitroquinoxaline -2,3(1H,4H)-dione were dissolved in 300 ml of tetrahydrofuran/methanol/dimethylformamide (3:3:1) and, after addition of 3 g of palladium/carbon (10%), hydrogenated. The mixture was filtered, the carbon was washed with methanolic ammonia solution, and the combined filtrates were concentrated under reduced pressure. The residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1). 2.2 g (8%) of product el and 18.5 g (80%) of product e2 were obtained.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. washthe carbon was washed with methanolic ammonia solution
  3. concentrationthe combined filtrates were concentrated under reduced pressure
  4. customThe residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1)

Quellen und Nachweise

ORD-Eintrag
ord-2cabe931f87a4b0aae7e47fa42588839
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05849743

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