Trifluoroacetic acid → 5-(3-Methoxy-allylidene)-1,3-dimethyl-pyrimidine-2,4,6-trione

HRID 76821

Reaktionsgleichung

Reaktionsgleichung von HRID 76821
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=[O:7])[N:5]([CH3:11])[C:3]1=[O:4].[CH3:12][O:13][CH:14](OC)[CH2:15][CH:16](OC)OC.FC(F)(F)C(O)=O>>[CH3:12][O:13][CH:14]=[CH:15][CH:16]=[C:8]1[C:9](=[O:10])[N:2]([CH3:1])[C:3](=[O:4])[N:5]([CH3:11])[C:6]1=[O:7]

Komponenten

4

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

1,3-Dimethylbarbituric acid (20 g, 0.1 mol; Aldrich) was placed in 100 mL round-bottom one-necked flask equipped with magnetic stir bar and reflux condenser, 1,1,3,3-tetramethoxy-propane, (40 mL, 0.2 mol; Aldrich) and 1 mL of Trifluoroacetic Acid (2 mL, 0.03 mol; Sigma) were added to the reaction mixture. The flask was heated at 100° C. with stirring for 5 hours and then cooled to room temperature. The crystallized product was filtered, washed with methanol and dried. The yield was 23 g (80% of theory).

Aufarbeitung

  1. customequipped with magnetic stir bar
  2. temperaturereflux condenser
  3. temperaturecooled to room temperature
  4. filtrationThe crystallized product was filtered
  5. washwashed with methanol
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-083eb0ef8a61487aa5f4542b7ed912c4
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835632B2

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