Phosphorus oxychloride → 5,8-Dichloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

HRID 1833344Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1833344
[Cl:1][C:2]1[N:16]=[CH:15][C:5]2[C:6](=O)[NH:7][C:8]3[N:9]([N:10]=[C:11]([CH3:13])[CH:12]=3)[C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:6]1[C:5]2[CH:15]=[N:16][C:2]([Cl:1])=[CH:3][C:4]=2[N:9]2[N:10]=[C:11]([CH3:13])[CH:12]=[C:8]2[N:7]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 1360252228-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one

Produkt 1

HCID 213891765,8-Dichloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

Versuchsvorschrift

23.5 g. of 8-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one of Example 1b are refluxed in 100 ml. of phosphorus oxychloride for 12 hours. The excess phosphorus oxychloride is distilled off in vacuo and the oily residue is poured on ice. After standing for 1 hour, 5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 17 g. (67%); m.p. 203.4° (ethyl acetate).

Aufarbeitung

  1. distillationThe excess phosphorus oxychloride is distilled off in vacuo
  2. additionthe oily residue is poured on ice
  3. filtration5,8-dichloro2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off

Quellen und Nachweise

ORD-Eintrag
ord-7e2fc4a868fb42398ae8234a58fe9b1c
Quelldatensatz
uspto-grants-1978_01
Patentnummer
US04066645

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