Chloroform → 2-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile

HRID 904549Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 904549
[CH3:1][C:2]1[S:10][C:9]2[C:8](=[O:11])[N:7]3[CH:12]=[C:13]([C:16]([NH2:18])=O)[CH:14]=[CH:15][C:6]3=[N:5][C:4]=2[CH:3]=1.P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>N1C=CC=CC=1>[CH3:1][C:2]1[S:10][C:9]2[C:8](=[O:11])[N:7]3[CH:12]=[C:13]([C:16]#[N:18])[CH:14]=[CH:15][C:6]3=[N:5][C:4]=2[CH:3]=1

Komponenten

5

Edukt 3

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 129530542-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxamide

Produkt 1

HCID 129530552-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2-Methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxamide (Example 44), 0.6 g (0.0023 mol), in 10 ml of pyridine, 25 ml of phosphorus oxychloride and 25 ml of chloroform is refluxed on a steam bath for three hours. The solvents are evaporated in vacuo and the residue is treated with 100 ml of ice water. The resulting precipitate is filtered to give 0.5 g of 2-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile; mp 258°-259° C. after recrystallization from methanol.

Aufarbeitung

  1. customThe solvents are evaporated in vacuo
  2. additionthe residue is treated with 100 ml of ice water
  3. filtrationThe resulting precipitate is filtered

Quellen und Nachweise

ORD-Eintrag
ord-b688e56e8ad04bd9b90463a3645a4553
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04230707

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