Oxalic Acid → HCID 135577947, Verbindung

HRID 1638602Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1638602
C(O)(=O)C(O)=O.C(C(CC)C(O)=O)C.[C:15]([NH:18][C:19]1[NH:20][C:21](=[O:35])[C:22]([CH2:32][CH:33]=[O:34])=[C:23]([N:25]([C:29](=[O:31])[CH3:30])[C:26](=[O:28])[CH3:27])[N:24]=1)(=[O:17])[CH3:16].C(=O)(O)[O-].[Na+]>ClCCl>[C:15]([NH:18][C:19]1[NH:20][C:21](=[O:35])[C:22]([CH2:32][CH:33]=[O:34])=[C:23]([N:25]([C:29](=[O:31])[CH3:30])[C:26](=[O:28])[CH3:27])[N:24]=1)(=[O:17])[CH3:16]

Komponenten

5

Edukt 3

HCID 971Oxalic AcidHCID 516892Sodium BicarbonateHCID 136364561HCID 136364561, Verbindung

Produkt 1

HCID 135577947HCID 135577947, VerbindungAusbeute 46,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A slurry of Silica Gel 60 (6.0 g, Merck μ7734, 70-230 mesh) and aqueous oxalic acid (10%) (0.6 ml) in dichlormethane (12 ml) was stirred for 15 minutes. 2-(2-acetylamino-4-diacetylamino-1,6-dihydro-6-oxo-5-pyrimidinyl)acetaldehyde diethyl acetate (1.0 g, 2.7 mmol) was added and the mxiture was stirred for 18 hours. Sodium bicarbonate (0.2 g, 2.4 mmol) was added and after 10 minutes the slurry was filtered and washed with ethyl acetate. The filtrates and wash were combined and spin evaporated in vacuo to give 0.37 g (46% of theory) of 2-(2-acetylamino-4-diacetylamino-1,6-dihydro-6-oxo-5-pyrimidinyl)acetaldehyde. The analytical sample was prepared by recrystallization from acetone to give 0.21 g (26% of theory), mp 169°-170° C.)

Aufarbeitung

  1. filtrationwas filtered
  2. washwashed with ethyl acetate
  3. washThe filtrates and wash
  4. customspin evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-387658a6e6634f79b48bc3e69c86a6d4
Quelldatensatz
uspto-grants-1989_11
Patentnummer
US04880812

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