Phosphorus pentachloride → 927-92-4

HRID 397714Notes

Reaction equation

HRID 397714 reaction equation
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[CH2:7]([S:14]([OH:17])(=O)=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[Na]>>[CH2:7]([S:14]([Cl:2])(=[O:17])=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

Participants

4

Reactant 3

HCID 24819Phosphorus pentachlorideHCID 898291-Heptanesulfonic acidHCID 5360545Sodium

Product 1

HCID 10878141927-92-4

Procedure

To phosphorous pentachloride (3.3 g, 16 mmol) was added solid heptanesulfonic acid, sodium salt monohydrate (1.75 g, 8 mmol) and the mixture was left to stir overnight under nitrogen. Phosphorous oxychloride was removed by distillation at 150° C. for 3 h. The residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C. to give ca. 1 g of material which was allowed to cool to room temperature. The precipitated free acid was removed by filtration to afford the title compound as an oil (500 mg, 31%) which was used without further purification.

Workup

  1. waitthe mixture was left
  2. customPhosphorous oxychloride was removed by distillation at 150° C. for 3 h
  3. distillationThe residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C.

Sources & evidence

ORD record
ord-99f74e0b64e84e4dad4737a1816ed3d2
Source dataset
uspto-grants-2003_08
Patent number
US06610711B2

Reaction notes

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