Phosphorus oxychloride → HCID 13309912, compound

HRID 325447Notes

Reaction equation

HRID 325447 reaction equation
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[NH:12][C:11](=O)[C:10]=12)=[O:5])[CH3:2].P(Cl)(Cl)([Cl:22])=O>>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12]=[C:11]([Cl:22])[C:10]=12)=[O:5])[CH3:2]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 13309870HCID 13309870, compound

Product 1

HCID 13309912HCID 13309912, compoundYield 47%

Procedure

4-Oxo-4,5-dihydroimidazo[1,5-a]quinoxaline 3-carboxylic acid ethyl ester (9 g) was suspended in 200 ml of phosphorus oxychloride and the mixture was heated with stirring until it became a clear solution. After cooling to room temperature, the solution was concentrated under vacuum. The residual oil was taken up in chloroform and was put through a short silica gel dry column (chloroform as eluant). The product was obtained from column as an off-white colored solid (4.5 g, 47% yield), m.p. 128°-130° C.

Workup

  1. temperaturethe mixture was heated
  2. concentrationthe solution was concentrated under vacuum
  3. dry with materialdry column (chloroform as eluant)

Sources & evidence

ORD record
ord-ee3ddaf138624df0a32bee6c0206ab65
Source dataset
uspto-grants-1984_04
Patent number
US04440929

Reaction notes

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