Phosphorus oxychloride → 2,5-Dichloropyrido[3,4-b]pyrazine

HRID 1526550

Reaktionsgleichung

Reaktionsgleichung von HRID 1526550
[Cl:1][C:2]1[C:7]2[N:8]=[CH:9][C:10](=O)[NH:11][C:6]=2[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:10]1[N:11]=[C:6]2[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[C:7]2=[N:8][CH:9]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 867157425-Chloropyrido[3,4-b]pyrazin-2(1H)-one

Produkt 1

HCID 867157432,5-Dichloropyrido[3,4-b]pyrazineAusbeute 92,4 %

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A suspension of 5-chloropyrido[3,4-b]pyrazin-2(1H)-one (0.57 g, 3.14 mmol) in phosphorus oxychloride (10.24 mL, 110 mmol) was stirred at 110° C. for two hours, and then concentrated. The residue was dissolved in DCM, washed with saturated sodium bicarbonate, dried over anhydrous sodium sulfate, filtered, and concentrated to afford the title compound (580 mg, 2.90 mmol). MS m/z=200 (M+H)+.

Aufarbeitung

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in DCM
  3. washwashed with saturated sodium bicarbonate
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-6c7a4e1e071b48d9854d192ec089b962
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085576B2

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