Phosphorus oxychloride → HCID 136079766, compound

HRID 2418775Notes

Reaction equation

HRID 2418775 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([S:19]([O-:22])(=O)=[O:20])[CH:5]=[CH:6][C:7]=1[N:8]=[N:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([C:17]#[N:18])[CH:11]=1.[Na+].P(Cl)(Cl)([Cl:26])=O.CN(C)C(=O)C>C(#N)C>[CH3:1][C:2]1[CH:3]=[C:4]([S:19]([Cl:26])(=[O:22])=[O:20])[CH:5]=[CH:6][C:7]=1[N:8]=[N:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([C:17]#[N:18])[CH:11]=1

Participants

5

Reactant 3

HCID 24813Phosphorus oxychlorideHCID 31374DimethylacetamideHCID 136399294HCID 136399294, compound

Product 1

HCID 136079766HCID 136079766, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

12.5 g (0.037 mol) of the sodium benzenesulfonate obtained in Step (a) above was stirred in 74 ml of acetonitrile, to which were added dropwise 14 ml of phosphorus oxychloride and then 14 mol of N,N-dimethylacetamide, and the mixture was heated at 50° C. with stirring for 1.5 hours. After cooling, the reaction mixture was added to 300 ml of ice water and the crystals thus-precipitated were collected by filtration. Yield: 11.9 g (96%).

Workup

  1. temperatureAfter cooling
  2. customthe crystals thus-precipitated
  3. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-5271dfc3fbab4e75909ebef0717986fc
Source dataset
uspto-grants-1984_09
Patent number
US04473632

Reaction notes

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