Phosphorus oxychloride → 2,6-Dichloroquinoxaline

HRID 1380467Notes

Reaction equation

HRID 1380467 reaction equation
O[C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:12])[CH:8]=2)[N:3]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:12])[CH:8]=2)[N:3]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178516724HCID 178516724, compound

Product 1

HCID 877482,6-Dichloroquinoxaline

Procedure

45 g of 2-hydroxy-6-chloroquinoxaline are treated in a sulphonation flask with 100 ml of phosphorus oxychloride. The mixture is stirred at reflux temperature for 20 minutes. The excess phosphorus oxychloride is thereupon distilled off and the residue is treated with 500 ml of ice-water. The product obtained is filtered off and washed with water until it is neutral. By crystallization from ethanol/water there is obtained 2,6-dichloroquinoxaline of melting point 152° C.

Workup

  1. temperatureat reflux temperature for 20 minutes
  2. distillationThe excess phosphorus oxychloride is thereupon distilled off
  3. additionthe residue is treated with 500 ml of ice-water
  4. customThe product obtained
  5. filtrationis filtered off
  6. washwashed with water until it
  7. customBy crystallization from ethanol/water there

Sources & evidence

ORD record
ord-14819dabc4ab47d3a702cc75653d95fa
Source dataset
uspto-grants-1986_04
Patent number
US04582526

Reaction notes

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