Reaktion #484896

Reaktionsgleichung

phosphorous pentachloride

heptanesulfonic acid

sodium

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material

n-Heptanesulfonyl Chloride

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle