Phosphorus oxychloride → HCID 13562763, compound

HRID 973817Notes

Reaction equation

HRID 973817 reaction equation
O[C:2]1[N:7]2[N:8]=[C:9]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[N:10]=[C:6]2[N:5]=[C:4]([CH3:16])[CH:3]=1.P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[N:10]=[C:6]2[N:5]=[C:4]([CH3:16])[CH:3]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178499620HCID 178499620, compound

Product 1

HCID 13562763HCID 13562763, compound

Procedure

A solution of the product obtained in Step 3 (1.5 g) in 15 ml of phosphorus oxychloride was refluxed for two hours, excess phosphorus oxychloride was distilled off, the residue was dissolved in chloroform, and the solution was washed with ice water. After removing the solvent from the organic layer under reduced pressure, the residue was purified by silica gel chromatography, affording 1 g of the objective compound.

Workup

  1. distillationexcess phosphorus oxychloride was distilled off
  2. dissolutionthe residue was dissolved in chloroform
  3. washthe solution was washed with ice water
  4. customAfter removing the solvent from the organic layer under reduced pressure
  5. customthe residue was purified by silica gel chromatography

Sources & evidence

ORD record
ord-f0c2cf4821db41a4b7d44f628e25236b
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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