Morpholine → (6-Nitro-7-morpholino-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester

HRID 618642Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 618642
[CH2:1]([O:3][P:4]([CH2:9][N:10]1[C:19]2[C:14](=[CH:15][C:16]([N+:21]([O-:23])=[O:22])=[C:17](F)[CH:18]=2)[NH:13][C:12](=[O:24])[C:11]1=[O:25])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[NH:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1>>[CH2:1]([O:3][P:4]([CH2:9][N:10]1[C:19]2[C:14](=[CH:15][C:16]([N+:21]([O-:23])=[O:22])=[C:17]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)[CH:18]=2)[NH:13][C:12](=[O:24])[C:11]1=[O:25])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2]

Komponenten

3

Edukt 2

HCID 8083MorpholineHCID 17800809(6-Nitro-7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester

Produkt 1

HCID 17800789(6-Nitro-7-morpholino-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl esterAusbeute 181,8 %

Versuchsvorschrift

140 mg of (6-nitro-7-fluoro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester is heated with 129 mg of morpholine for 1.5 hours to 120° C. bath temperature. After concentration by evaporation in a vacuum, the residue is chromatographed on silica gel with toluene:glacial acetic acid:water=10:10:1. After concentration by evaporation of the corresponding fractions, 300 mg of (7-morpholino-6-nitro-1,2,3,4-tetrahydro-2,3-dioxoquinoxalin-1-yl)methanephosphonic acid diethyl ester is obtained.

Aufarbeitung

  1. concentrationAfter concentration
  2. customby evaporation in a vacuum
  3. customthe residue is chromatographed on silica gel with toluene
  4. concentrationAfter concentration
  5. customby evaporation of the corresponding fractions

Quellen und Nachweise

ORD-Eintrag
ord-668f7d6b42e344dda9eb1a4cae6ea60a
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05955461

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