Methyl (7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonate → Bis(p-tert-butylphenyl)iodonium camphorsulfonate

HRID 1168010Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1168010
[Cl-].[C:2]([C:6]1[CH:11]=[CH:10][C:9]([I+:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:15][CH:14]=2)=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3].[C:23]12([CH2:33][S:34]([O:37]C)(=[O:36])=[O:35])[C:30]([CH3:32])([CH3:31])[CH:27]([CH2:28][CH2:29]1)[CH2:26][C:24]2=[O:25]>C(OCC)(=O)C>[C:23]12([CH2:33][S:34]([O-:37])(=[O:35])=[O:36])[C:30]([CH3:32])([CH3:31])[CH:27]([CH2:28][CH2:29]1)[CH2:26][C:24]2=[O:25].[C:19]([C:16]1[CH:17]=[CH:18][C:13]([I+:12][C:9]2[CH:8]=[CH:7][C:6]([C:2]([CH3:5])([CH3:4])[CH3:3])=[CH:11][CH:10]=2)=[CH:14][CH:15]=1)([CH3:22])([CH3:21])[CH3:20]

Komponenten

4

Edukt 2

HCID 573022Methyl (7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonateHCID 21889439Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, chloride

Produkt 1

HCID 21930728Bis(p-tert-butylphenyl)iodonium camphorsulfonateAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Ethyl acetate (50 ml) was added to bis(p-tert-butylphenyl)iodonium chloride (17.06 g; 39.79 mmol) and methyl camphorsulfonate (10.78 g; 43.76 mmol). The resultant mixture was heated at 77° C.-80° C. and refluxed for 24 hours while being stirred. The reaction mixture was cooled, and formed solid was removed through filteration. The solid was recrystallized from acetone, and dried under vacuum, to thereby yield 20.63 g of bis(p-tert-butylphenyl)iodonium camphorsulfonate (yield: 83%).

Aufarbeitung

  1. temperaturerefluxed for 24 hours
  2. temperatureThe reaction mixture was cooled
  3. customformed solid
  4. customwas removed through filteration
  5. customThe solid was recrystallized from acetone
  6. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-68e48a9ec25440429ec7d5eaec7e954d
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06620957B1

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