Phosphorus oxychloride → HCID 22011950, Verbindung

HRID 566389Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 566389
[CH3:1][C:2]1[O:6][C:5]([C:7]2[N:17]=[CH:16][C:10]3[N:11]=[CH:12][NH:13][C:14](=O)[C:9]=3[CH:8]=2)=[N:4][N:3]=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:14]1[C:9]2[CH:8]=[C:7]([C:5]3[O:6][C:2]([CH3:1])=[N:3][N:4]=3)[N:17]=[CH:16][C:10]=2[N:11]=[CH:12][N:13]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 135817447HCID 135817447, Verbindung

Produkt 1

HCID 22011950HCID 22011950, Verbindung

Versuchsvorschrift

6-(5-Methyl-1,3,4-oxadiazol-2-yl)-pyrido[3,4-d]pyrimidin-4-one (0.5 g) was treated with phosphorus oxychloride at room temperature under N2. After 1 hour at room temperature and 1 hour at 50° C., the mixture was concentrated in vacuo, azeotroping with toluene, then taken up in ethyl acetate, washed with sodium bicarbonate solution, dried and concentrated in vacuo to give the title compound (0.17 g) as an orange solid; δH CDCl3 9.68 (1H,s), 9.30 (1H,s), 8.96 (1H,s), 2.75 (3H,s); m/z (M+1+)248.

Aufarbeitung

  1. concentration1 hour at 50° C., the mixture was concentrated in vacuo
  2. customazeotroping with toluene
  3. washwashed with sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8a0d1750a8984fbcacad836ffbe7c7ed
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06174889B1

Notizen zur Reaktion

Wird geladen…