Malonamide → HCID 178513675, Verbindung

HRID 1020806

Reaktionsgleichung

Reaktionsgleichung von HRID 1020806
CN1[CH:7]=[CH:6][C:5](=[O:8])N(C)C1=O.[C:11]([NH2:17])(=[O:16])[CH2:12][C:13]([NH2:15])=[O:14].[O-]CC.[Na+]>CCO>[OH:14][C:13]1[N:15]=[C:5]([OH:8])[CH:6]=[CH:7][C:12]=1[C:11]([NH2:17])=[O:16]

Komponenten

5

Edukt 3

HCID 7911MalonamideHCID 701221,3-DimethyluracilHCID 2723922Sodium ethoxide

Produkt 1

HCID 178513675HCID 178513675, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of compound 1,3-dimethylpyrimidine-2,4(1H,3H)-dione (14 g, 0.1 mol), malonamide (45 g, 0.44 mol) and sodium ethoxide (34 g, 0.4 mol) in EtOH (500 mL) was refluxed for 20 mins. The mixture was cooled to r.t, quenched by water and acidified with 1 M HCl to pH=1-2. The solid was filtered and the filter cake was concentrated in vacuo to afford compound 2,6-dihydroxynicotinamide. (10 g, yield: 65%). 1H-NMR (400 MHz, DMSO-d6) δ (ppm) 7.90-7.88 (d, 1H), 5.66-5.64 (d, 1H).

Aufarbeitung

  1. temperaturewas refluxed for 20 mins
  2. temperatureThe mixture was cooled
  3. customquenched by water
  4. filtrationThe solid was filtered
  5. concentrationthe filter cake was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9591e8f4d4994c639c588edce3d4aefc
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08716478B2

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