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

HRID 1155897Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1155897
[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.N1C=CC=CC=1.P(Cl)(Cl)(Cl)=O>C(Cl)(Cl)Cl>[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 1049PyridineHCID 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 6212ChloroformLösungsmittel

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 of pyridine, 25 ml of phosphorous 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-9d869a94cbc04e69993ce8a74ac79d11
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04332947

Notizen zur Reaktion

Wird geladen…