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

HRID 1168013노트

반응식

HRID 1168013 반응식
C([O-])(=O)C.[C:5]([C:9]1[CH:14]=[CH:13][C:12]([I+:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:18][CH:17]=2)=[CH:11][CH:10]=1)([CH3:8])([CH3:7])[CH3:6].[C:26]12([CH2:36][S:37]([O:40]C)(=[O:39])=[O:38])[C:33]([CH3:35])([CH3:34])[CH:30]([CH2:31][CH2:32]1)[CH2:29][C:27]2=[O:28]>C(OCC)(=O)C>[C:26]12([CH2:36][S:37]([O-:40])(=[O:38])=[O:39])[C:33]([CH3:35])([CH3:34])[CH:30]([CH2:31][CH2:32]1)[CH2:29][C:27]2=[O:28].[C:22]([C:19]1[CH:20]=[CH:21][C:16]([I+:15][C:12]2[CH:11]=[CH:10][C:9]([C:5]([CH3:8])([CH3:7])[CH3:6])=[CH:14][CH:13]=2)=[CH:17][CH:18]=1)([CH3:25])([CH3:24])[CH3:23]

참가 물질

4

반응물 2

HCID 573022Methyl (7,7-dimethyl-2-oxobicyclo[2.2.1]heptan-1-yl)methanesulfonateHCID 21909498Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, acetate

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Ethyl acetate (50 ml) was added to bis(p-tert-butylphenyl)iodonium acetate (467 mg; 1 mmol) and methyl camphorsulfonate (259 mg; 1.05 mmol). The resultant mixture was refluxed for 24 hours while being stirred. The reaction mixture was cooled, and formed solid was removed through filtration. The solid was recrystallized from acetone, and dried under vacuum, to thereby yield 518 mg of bis(p-tert-butylphenyl)iodonium camphorsulfonate (yield: 83%).

후처리

  1. temperatureThe reaction mixture was cooled
  2. customformed solid
  3. customwas removed through filtration
  4. customThe solid was recrystallized from acetone
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-38c340f477e14924a15db84190af7c68
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620957B1

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