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

HRID 1168009ノート

反応式

HRID 1168009 の反応式
[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]

参加物

4

反応物 2

HCID 21889439Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, chlorideHCID 22995013Methyl 9,10-dimethoxyanthracene-2-sulfonate

生成物 1

HCID 22995016Bis(p-tert-butylphenyl)iodonium 9,10-dimethoxyanthracene-2-sulfonate収率 78%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ec9314f1770e4db9adb65ab246b6c79c
出典データセット
uspto-grants-2003_09
特許番号
US06620957B1

反応ノート

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