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

HRID 1833342Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1833342
[CH3:1][C:2]1[CH:15]=[C:5]2[NH:6][C:7](=O)[C:8]3[CH:13]=[N:12][CH:11]=[CH:10][C:9]=3[N:4]2[N:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:7]1[C:8]2[CH:13]=[N:12][CH:11]=[CH:10][C:9]=2[N:4]2[N:3]=[C:2]([CH3:1])[CH:15]=[C:5]2[N:6]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 1361423592-Methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidin-5(4H)-one

Produkt 1

HCID 213891855-Chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine

Versuchsvorschrift

200 g. of 2-methylpyrazolo[1,5-a]pyrido[3,4-e]-pyrimidin-5(4H)-one of Example 1c are refluxed with 800 ml. of phosphorus oxychloride overnight. The excess phosphorus oxychloride is removed in vacuo and the oily residue decomposed by pouring on ice. The acidic aqueous solution is made alkaline with sodium hydroxide. The precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off, yield: 143 g. (66%); m.p. 169.8° (ethyl acetate).

Aufarbeitung

  1. customThe excess phosphorus oxychloride is removed in vacuo
  2. additionby pouring on ice
  3. filtrationThe precipitated 5-chloro-2-methylpyrazolo[1,5-a]pyrido[3,4-e]pyrimidine is filtered off

Quellen und Nachweise

ORD-Eintrag
ord-17fc6805ef334857b62c9c421f655886
Quelldatensatz
uspto-grants-1978_01
Patentnummer
US04066645

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