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

HRID 930451Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 930451
[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-aa7383c7f17047ee8217fd130fbad691
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09296734B2

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