Phosphorus oxychloride → 4-Tert-butyl-6-chloropyrimidin-2-amine

HRID 619284Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 619284
[NH2:1][C:2]1[N:7]=[C:6](O)[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[NH2:1][C:2]1[N:7]=[C:6]([Cl:15])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[N:3]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178441204HCID 178441204, Verbindung

Produkt 1

HCID 218463784-Tert-butyl-6-chloropyrimidin-2-amine

Versuchsvorschrift

2-Amino-4-hydroxy-6-tert-butylpyrimidine (8.35 g) was dissolved in 50 mL of phosphorus oxychloride and the solution refluxed for 2 hours. Excess phosphorus oxychloride was removed under vacuum and the residue dissolved in 100 mL of ethanol. The solution was adjusted to pH 8 with ice-cold concentrated ammonium hydroxide, and solvent removed under reduced pressure. The residue was filtered to give a white solid, which was recrystallized from ethanol-water to give 2-amino-4-chloro-6-tert-butylpyrimidine (3.66 g), m.p. 87.7-88.9° C.

Aufarbeitung

  1. temperaturethe solution refluxed for 2 hours
  2. customExcess phosphorus oxychloride was removed under vacuum
  3. dissolutionthe residue dissolved in 100 mL of ethanol
  4. customremoved under reduced pressure
  5. filtrationThe residue was filtered
  6. customto give a white solid, which
  7. customwas recrystallized from ethanol-water

Quellen und Nachweise

ORD-Eintrag
ord-bf91c58415d0425b95f75d8b7891b757
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05958934

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