Dichloromethane → HCID 18362461, 화합물

HRID 381205

반응식

HRID 381205 반응식
[S:1]([C:5]([C:8]([C:11]([C:14]([F:17])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([O-:4])(=[O:3])=[O:2].[K+].S([O-])(O)(=O)=O.[CH3:24][C:25]1[CH:30]=[CH:29][C:28]([I+:31][C:32]2[CH:37]=[CH:36][C:35]([CH2:38][CH:39]([CH3:41])[CH3:40])=[CH:34][CH:33]=2)=[CH:27][CH:26]=1.C(Cl)Cl>O.CO>[S:1]([C:5]([C:8]([C:11]([C:14]([F:15])([F:16])[F:17])([F:12])[F:13])([F:10])[F:9])([F:7])[F:6])([O-:4])(=[O:3])=[O:2].[CH3:24][C:25]1[CH:26]=[CH:27][C:28]([I+:31][C:32]2[CH:37]=[CH:36][C:35]([CH2:38][CH:39]([CH3:41])[CH3:40])=[CH:34][CH:33]=2)=[CH:29][CH:30]=1

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 23675274Potassium perfluorobutanesulfonateHCID 86591397HCID 86591397, 화합물

생성물 1

HCID 18362461HCID 18362461, 화합물수율 34.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

4.5 g of potassium nonaflate is suspended in 15 ml of water. To the solution is added 4.93 g of the crude (4-methylphenyl)(4′-isobutylphenyl)iodonium hydrogensulfate dissolved in 10 ml of methanol. The mixture is stirred for 1 hour at room temperature. 15 ml of methylene chloride is added to the solution and stirred overnight at room temperature. The product is extracted with methylene chloride and the organic layer is washed with water, dried over MgSO4, and concentrated. The residue is purified by flash chromatography on silica gel with methylene chloride and ethanol (95:5) as eluent, yielding 2.46 g (3.8 mmol; 34%) of (4-methylphenyl)(4′-isobutylphenyl)iodonium nonaflate as a brown resin. The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ [ppm]: 0.88 (d, 6H), 1.84 (m,1H), 2.41 (s, 3H), 2.50 (d, 2H), 7.21-7.26 (m, 4H), 7.84 (d, 4H). Elemental analysis: calculation for C21H20O3F9SI

후처리

  1. stirringstirred overnight at room temperature
  2. extractionThe product is extracted with methylene chloride
  3. washthe organic layer is washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue is purified by flash chromatography on silica gel with methylene chloride and ethanol (95:5) as eluent

출처 및 근거

ORD 기록
ord-b1f4c4838e314a28833b44c048f8935a
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06306555B1

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