Phosphorus oxychloride → 2-Chloro-5,6,7,8-tetrahydroquinoxaline

HRID 1789996Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1789996
[NH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[N:4]=[CH:3][C:2]1=O.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:2]1[CH:3]=[N:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[N:1]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 8202241,2,5,6,7,8-Hexahydroquinoxalin-2-one

Produkt 1

HCID 220369342-Chloro-5,6,7,8-tetrahydroquinoxalineAusbeute 86 %

Versuchsvorschrift

A mixture of 5,6,7,8-tetrahydro-2(1H)-quinoxalinone in phosphoryl chloride (200 ml) was stirred and refluxed for 3 hours. The solvent was evaporated. The residue was taken up in ice and CH2Cl2. The mixture was basified with NH4OH. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated, yielding 34 g (86%) of 2-chloro-5,6,7,8-tetrahydroquinoxaline (interm. 3).

Aufarbeitung

  1. temperaturerefluxed for 3 hours
  2. customThe solvent was evaporated
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-fbaa14d6e4c243d89586713fa1c24c59
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07071192B1

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