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

HRID 48207Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 48207
[Br:1][C:2]1[CH:3]=[C:4]([NH2:14])[C:5]([NH2:13])=[C:6]2[C:11]=1[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7]2.[C:15](O)(=[O:19])[C:16](O)=[O:17]>Cl>[Br:1][C:2]1[C:11]2[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7][C:6]=2[C:5]2[NH:13][C:15](=[O:19])[C:16](=[O:17])[NH:14][C:4]=2[CH:3]=1

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 103550328-Bromo-1,2,3,4-tetrahydro-2-methyl-5,6-isoquinolinediamine

Produkt 1

HCID 98181346-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dioneAusbeute 24,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of the product from Example 13 (0.62 g, 2.56 mmol) and oxalic acid (0.23 g, 2.56 mmol) in 25 mL of 3N aqueous HCl solution were heated at reflux for 18 hours. The reaction mixture was cooled to room temperature and the solid which formed was collected by filtration and washed with cold water. The solid was recrystallized from hot water and dried under vacuum (100° C., P2O5) to give the title compound as a tan solid (0.191 g, 20%), mp=315-320° C. (dec.).

Aufarbeitung

  1. temperatureat reflux for 18 hours
  2. customthe solid which formed
  3. filtrationwas collected by filtration
  4. washwashed with cold water
  5. customThe solid was recrystallized from hot water
  6. dry with materialdried under vacuum (100° C., P2O5)

Quellen und Nachweise

ORD-Eintrag
ord-28485785eeb5490989bcf2076b9474c3
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06703391B2

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