Phosphorus oxychloride → HCID 22341136, Verbindung

HRID 584682Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 584682
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=O)[C:6]([CH2:14][CH2:15][CH2:16][Cl:17])=[N:5]2.O=P(Cl)(Cl)[Cl:20]>>[Cl:20][C:7]1[C:6]([CH2:14][CH2:15][CH2:16][Cl:17])=[N:5][C:4]2[C:9](=[CH:10][C:11]([Cl:12])=[C:2]([Cl:1])[CH:3]=2)[N:8]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 22341064HCID 22341064, Verbindung

Produkt 1

HCID 22341136HCID 22341136, VerbindungAusbeute 21 %

Versuchsvorschrift

6,7-Dichloro-3-(3-chloropropyl)-1H-quinoxalin-2-one (0.68 g, 2.33 mmol) was added to POCl3 (10 ml) and the resulting mixture was heated under reflux for 0.5 hours. The reaction mixture was poured onto ice and extracted with dichloromethane (3×). The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporate in vacuo. The resulting oil was purified by flash column chromatography (dichloromethane) to yield 21% of 2,6,7-trichloro-3-(3-chloropropyl)quinoxaline as a colourless oil.

Aufarbeitung

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 0.5 hours
  3. additionThe reaction mixture was poured onto ice
  4. extractionextracted with dichloromethane (3×)
  5. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporate in vacuo
  8. customThe resulting oil was purified by flash column chromatography (dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-2e3627308cef4a78801d6d5207f35d54
Quelldatensatz
uspto-grants-2005_08
Patentnummer
US06927214B1

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