Methanesulfonic Acid → 9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione Methanesulfonate

HRID 48226Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 48226
[CH2:1]([N:3]1[CH2:16][CH2:15][C:14]2[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][C:11]3[NH:10][C:9](=[O:20])[C:8](=[O:21])[NH:7][C:6]=3[C:5]=2[CH2:4]1)[CH3:2].[CH3:22][S:23]([OH:26])(=[O:25])=[O:24]>CN(C)C=O>[CH3:22][S:23]([OH:26])(=[O:25])=[O:24].[CH2:1]([N:3]1[CH2:16][CH2:15][C:14]2[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][C:11]3[NH:10][C:9](=[O:20])[C:8](=[O:21])[NH:7][C:6]=3[C:5]=2[CH2:4]1)[CH3:2]

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 10266209(9S)-9-ethyl-3-hydroxy-6-nitro-7,8,9,10-tetrahydropyrido[3,4-f]quinoxalin-9-ium-2-olate

Produkt 1

HCID 227424649-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione MethanesulfonateAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

The product from Example 74 was suspended in 300 mL dimethylformamide and 1 mL of 3 N methanesulfonic acid added. The suspension was warmed to 100° C. The colour changed from orange to yellow and all of the solid dissolved. Solvent was evaporated in vacuo, the yellow residue washed with acetone and then dried under vacuum over P2O5 to give the title compound (0.73 g, 92% yield) mp=302-304° C.

Aufarbeitung

  1. dissolutiondissolved
  2. customSolvent was evaporated in vacuo
  3. washthe yellow residue washed with acetone
  4. dry with materialdried under vacuum over P2O5

Quellen und Nachweise

ORD-Eintrag
ord-da20f6b9c3c44a1780128c8672b4caa0
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06703391B2

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