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

HRID 2057133노트

반응식

HRID 2057133 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ba9b3f66129459398daca0bb5411a10
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07335787B2

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