Ammonia → 4-Chloro-2-(4-methoxyphenyl)-6-methylpyrimidine

HRID 1082083

Reaktionsgleichung

Reaktionsgleichung von HRID 1082083
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[N:3]=1.N.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[N:3]=1

Komponenten

4

Edukt 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 178488949HCID 178488949, Verbindung

Produkt 1

HCID 153834554-Chloro-2-(4-methoxyphenyl)-6-methylpyrimidine

Versuchsvorschrift

6.5 g of 4-hydroxy-2-(4-methoxyphenyl)-6-methylpyrimidine prepared in reference example 1 (3) was added to 30 ml of phosphorus oxychloride, and the mixture was refluxed with stirring for 30 minutes. The reaction mixture was cooled and poured into diluted ammonia solution and the precipitated crystals were filtered off. The crystals were dissolved in chloroform. After the chloroform layer was washed twice with water, it was dried with anhydrous magnesium sulfate and was evaporated in vacuo. The residue was crystallized with n-hexane and filtered off. Whereby 5.1 g of crystals was obtained. Melting point is 80° to 81° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe precipitated crystals were filtered off
  4. dissolutionThe crystals were dissolved in chloroform
  5. washAfter the chloroform layer was washed twice with water, it
  6. dry with materialwas dried with anhydrous magnesium sulfate
  7. customwas evaporated in vacuo
  8. customThe residue was crystallized with n-hexane
  9. filtrationfiltered off

Quellen und Nachweise

ORD-Eintrag
ord-c69c4e3abc1f456ebb318ed87e442425
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05589477

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