Phosphorus oxychloride → 4-Chloro-5-methyl-2-(methylsulfanyl)pyrimidine

HRID 1514406

Reaktionsgleichung

Reaktionsgleichung von HRID 1514406
[CH3:1][C:2]1[C:3](=O)[NH:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.O=P(Cl)(Cl)[Cl:13]>O1CCOCC1>[Cl:13][C:3]1[C:2]([CH3:1])=[CH:7][N:6]=[C:5]([S:8][CH3:9])[N:4]=1

Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 2405755-Methyl-2-(methylthio)pyrimidin-4(3H)-one

Produkt 1

HCID 235627084-Chloro-5-methyl-2-(methylsulfanyl)pyrimidineAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 5-methyl-2-methylsulfanyl-3H-pyrimidin-4-one (6.86 g, 44 mmol) and POCl3 (14 ml) in dioxane (60 ml) was refluxed for 2 hours. The solvent was removed under vacuum and the residue was quenched with ice and extracted with diethylether. The organic phase was dried (Na2SO4) and evaporated to give 6.8 g of the title compound as oil that was used in the next step without further purification. (89% yield)

Aufarbeitung

  1. temperaturewas refluxed for 2 hours
  2. customThe solvent was removed under vacuum
  3. customthe residue was quenched with ice
  4. extractionextracted with diethylether
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-3d097722860d4ba3a29d4cf7f1820570
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08222266B2

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