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

HRID 1168010

반응식

HRID 1168010 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].[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]

참가 물질

4

반응물 2

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

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 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%).

후처리

  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

출처 및 근거

ORD 기록
ord-68e48a9ec25440429ec7d5eaec7e954d
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620957B1

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