Phosphorus oxychloride → 4,7-Dichloropyrido[3,2-d]pyrimidine

HRID 1526558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1526558
[Cl:1][C:2]1[CH:11]=[N:10][C:9]2[C:8](=O)[N:7]=[CH:6][NH:5][C:4]=2[CH:3]=1.CCN(C(C)C)C(C)C.P(Cl)(Cl)([Cl:24])=O>C1(C)C=CC=CC=1>[Cl:24][C:8]1[C:9]2[N:10]=[CH:11][C:2]([Cl:1])=[CH:3][C:4]=2[N:5]=[CH:6][N:7]=1

Komponenten

5

Edukt 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 1785182197-chloro-1H-pyrido[3,2-d]pyrimidin-4-one

Produkt 1

HCID 714284454,7-Dichloropyrido[3,2-d]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a mixture of 7-chloropyrido[3,2-d]pyrimidin-4(1H)-one (250 mg, 1.377 mmol) in toluene (12 mL) were added DIPEA (0.73 mL, 4.20 mmol) and phosphorus oxychloride (0.391 mL, 4.27 mmol), and the reaction was stirred at reflux for 1 hour. After cooling to RT, the reaction mixture was concentrated to provide the title compound. LC/MS (ESI+) m/z=200 (M+H)+.

Aufarbeitung

  1. temperatureat reflux for 1 hour
  2. concentrationthe reaction mixture was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-e0b1df88ef4e49cb9c77cec41a178fc8
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085576B2

Notizen zur Reaktion

Wird geladen…