Oxalic Acid → 6-Bromo-1,4,7,8,9,10-hexahydro-9-(2-phenylethyl)pyrido[3,4-f]quinoxaline-2,3-dione

HRID 1530841Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1530841
[Br:1][C:2]1[CH:11]=[C:10]([NH2:12])[C:9]([NH2:13])=[C:8]2[C:3]=1[CH2:4][CH2:5][N:6]([CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH2:7]2.[C:22](O)(=[O:26])[C:23](O)=[O:24]>Cl>[Br:1][C:2]1[C:3]2[CH2:4][CH2:5][N:6]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:7][C:8]=2[C:9]2[NH:13][C:22](=[O:26])[C:23](=[O:24])[NH:12][C:10]=2[CH:11]=1

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 155241925-Bromo-1,2,3,4-tetrahydro-2-(2-phenylethyl)-7,8-isoquinolinediamine

Produkt 1

HCID 155241936-Bromo-1,4,7,8,9,10-hexahydro-9-(2-phenylethyl)pyrido[3,4-f]quinoxaline-2,3-dioneAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of the product from Example 10 (0.54 g, 1.56 mmol) in 3N HCl (20 mL) was treated with oxalic acid (0.3 g, 2.34 mmol) and refluxed for four hours. When cool to room temperature the precipitate was filtered, suspended in water (70 mL) and basifyed to pH 10. The solids were filtered, and dried to give the title compound (0.37 g, 60%) as a brown solid, mp=290-295° C.

Aufarbeitung

  1. temperaturerefluxed for four hours
  2. filtrationwas filtered
  3. filtrationThe solids were filtered
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9a2009b991e44cad9973b61da79d0920
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06197771B1

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