Methanol → AB-323/25048145

HRID 1467831Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1467831
[N+:1]([C:4]1[C:5](=[O:14])[N:6]([CH3:13])[C:7](=[O:12])[N:8]([CH3:11])[C:9]=1[CH3:10])([O-])=O.CO>[Pd].C1(C)C=CC=CC=1>[NH2:1][C:4]1[C:5](=[O:14])[N:6]([CH3:13])[C:7](=[O:12])[N:8]([CH3:11])[C:9]=1[CH3:10]

Komponenten

5

Edukt 2

HCID 887MethanolHCID 7503695-Nitro-1,3,6-trimethyluracil

Produkt 1

HCID 816935AB-323/25048145Ausbeute 120,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a stirred suspension of 5-nitro-1,3,6-trimethylpyrimidine-2,4(1H,3H)-dione (4.2 g, 20.084 mmol) in 1:1 mixture of methanol and toluene (200 ml) was added 10% Pd—C (1.2 g). The reaction mixture was stirred under hydrogen atmosphere at room temperature overnight. The mixture was then filtered over a celite bed and was thoroughly washed with methanol (200 ml). The filtrate was collected and evaporated to give viscous residue which was then purified by column chromatography to afford 4.1 g of the product as an off-white solid.

Aufarbeitung

  1. filtrationThe mixture was then filtered over a celite bed
  2. washwas thoroughly washed with methanol (200 ml)
  3. customThe filtrate was collected
  4. customevaporated
  5. customto give viscous residue which
  6. customwas then purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-c3672729829a4f6fb418ad75ae54003a
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09000159B2

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