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

HRID 2057134ノート

反応式

HRID 2057134 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].[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9f60918b44c3468ab04076af3483a2c0
出典データセット
uspto-grants-2008_02
特許番号
US07335787B2

反応ノート

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