Water → 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

HRID 377609

Reaktionsgleichung

Reaktionsgleichung von HRID 377609
[CH3:1][N:2]1[C:9](=[O:10])[CH2:8][C:6](=O)[NH:5][C:3]1=[O:4].O.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[NH:5][C:3](=[O:4])[N:2]([CH3:1])[C:9](=[O:10])[CH:8]=1

Komponenten

4

Edukt 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 757221-Methyl-2,4,6(1H,3H,5H)-pyrimidinetrione

Produkt 1

HCID 961416-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

Versuchsvorschrift

1-Methylbarbituric acid (10 g) was suspended in phosphorus oxychloride (70 ml). Water (2 ml) was added and the mixture was heated at reflux for 40 minutes. The reaction was allowed to cool and was then concentrated under reduced pressure. The residue was poured onto a mixture of ice and water (200 ml). When the ice had melted, the precipitated solid was collected, washed with water and dried in vacuo at 50° C. to give the sub-title compound (6.86 g) as a yellow solid.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 40 minutes
  3. temperatureto cool
  4. concentrationwas then concentrated under reduced pressure
  5. additionThe residue was poured onto a mixture of ice and water (200 ml)
  6. customthe precipitated solid was collected
  7. washwashed with water
  8. customdried in vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-4b900d2df6f8472bb0082e6245023774
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06028074

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