HCID 10584109, Verbindung → HCID 10584991, Verbindung

HRID 1744765

Reaktionsgleichung

Reaktionsgleichung von HRID 1744765
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:7]=1[NH2:8].[CH:15](S([O-])(=O)=O)(O)[CH:16](S([O-])(=O)=O)O.O.[Na+].[Na+]>Cl>[CH2:9]([N:6]1[C:7]2[C:2](=[N:1][CH:15]=[CH:16][N:8]=2)[C:3](=[O:14])[NH:4][C:5]1=[O:13])[CH:10]([CH3:11])[CH3:12]

Komponenten

4

Edukt 2

HCID 10584109HCID 10584109, VerbindungHCID 16211366Disodium 1,2-dihydroxy-1,2-ethanedisulfonate monohydrate

Produkt 1

HCID 10584991HCID 10584991, VerbindungAusbeute 19,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

After dissolving 19.8 g (100 mmol) 5,6-diamino-1-isobutyluracil in 1 liter of 1N HCl at 70° C., 186.3 g of glyoxal sodium bisulfite addition compound hydrate was added and the mixture refluxed for 1 hour. After extracting the mixture several times with ethyl acetate, the collected ethyl acetate fractions were washed with water, dried over MgSO4 and evaporated. The crude product was purified by preparative column chromatography using chloroform/methanol 9:1 as eluant yielding 4.25 g (18%) of 1-isobutyl-1H-pteridine-2,4-dione (m.p. 200–201° C., Lit. 195–197° C.).

Aufarbeitung

  1. temperaturethe mixture refluxed for 1 hour
  2. extractionAfter extracting the mixture several times with ethyl acetate
  3. washthe collected ethyl acetate fractions were washed with water
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe crude product was purified by preparative column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-64f1a6ecd221468b9d26aa84a2812744
Quelldatensatz
uspto-grants-2006_03
Patentnummer
US07018786B2

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