(1,1'-Biphenyl)-4-sulfonic acid → (1,1'-Biphenyl)-4-sulphonyl chloride

HRID 378421Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 378421
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([S:7](O)(=[O:9])=[O:8])=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:19])=O>>[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([S:7]([Cl:19])(=[O:9])=[O:8])=[CH:3][CH:2]=1

Komponenten

3

Edukt 2

HCID 16673(1,1'-Biphenyl)-4-sulfonic acidHCID 24813Phosphorus oxychloride

Produkt 1

HCID 74192(1,1'-Biphenyl)-4-sulphonyl chlorideAusbeute 89,7 %

Versuchsvorschrift

4-Biphenylsulfonic acid (3.0 g, 12.8 mmol) was heated at 70° C. with phosphorus oxychloride (1.30 ml, 14.0 mol) for 2 h. Excess phosphorus oxychloride was removed under reduced pressure. The residue was decomposed with ice water and extracted with ethyl acetate. The extract was washed with 5% sodium bicarbinate solution, dried over anhydrous magnesium sulfate and concentrated to yield 2.9 g of crude 4-biphenylsulfonyl chloride.

Aufarbeitung

  1. customExcess phosphorus oxychloride was removed under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with 5% sodium bicarbinate solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fb9c566c900f4bc78da210375b5b0ec9
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06030991

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