Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, chloride → Bis(p-tert-butylphenyl)iodonium 9,10-dimethoxyanthracene-2-sulfonate

HRID 2057133

Reaktionsgleichung

Reaktionsgleichung von HRID 2057133
[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].[CH3:23][O:24][C:25]1[C:26]2[C:31]([C:32]([O:44][CH3:45])=[C:33]3[C:38]=1[CH:37]=[C:36]([S:39]([O:42]C)(=[O:41])=[O:40])[CH:35]=[CH:34]3)=[CH:30][CH:29]=[CH:28][CH:27]=2>C(#N)C>[CH3:23][O:24][C:25]1[C:26]2[C:31]([C:32]([O:44][CH3:45])=[C:33]3[C:38]=1[CH:37]=[C:36]([S:39]([O-:42])(=[O:40])=[O:41])[CH:35]=[CH:34]3)=[CH:30][CH:29]=[CH:28][CH:27]=2.[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

Versuchsvorschrift

Acetonitrile (90 ml) was added to bis(p-tert-butylphenyl)iodonium chloride (6.4 g; 15 mmol) and methyl 9,10-dimethoxyanthracene-2-sulfonate (6.48 g; 19.5 mmol). The resultant mixture was heated at 82° C.-85° C. and refluxed for 20 hours while being stirred. The reaction mixture was cooled, and precipitated solid was separated through filtration. The solid was washed with ethyl acetate, and dried under vacuum, to thereby yield 8.32 g of bis(p-tert-butylphenyl)iodonium 9,10-dimethoxyanthracene-2-sulfonate (yield: 78%). The chloride anion content of the resultant solid was 110 ppm, as determined by silver nitrate titration.

Aufarbeitung

  1. temperaturerefluxed for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. customprecipitated solid
  4. customwas separated through filtration
  5. washThe solid was washed with ethyl acetate
  6. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-3ba9b3f66129459398daca0bb5411a10
Quelldatensatz
uspto-grants-2008_02
Patentnummer
US07335787B2

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