Iodonium, diphenyl-, sulfate (1:1) → Diphenyliodonium phenylsulfate

HRID 585029노트

반응식

HRID 585029 반응식
S([O-])(O)(=O)=O.[C:6]1([I+:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[C:19]1([O:25][S:26]([O-:29])(=[O:28])=[O:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C[N+](C)(C)C>O>[C:19]1([O:25][S:26]([O-:29])(=[O:28])=[O:27])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1.[C:13]1([I+:12][C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

4

반응물 2

HCID 170803Iodonium, diphenyl-, sulfate (1:1)HCID 22338997Tetramethylammonium phenylsulfate

생성물 1

HCID 22339003Diphenyliodonium phenylsulfate수율 35.8%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

3 g of the crude diphenyliodonium hydrogensulfate are dissolved in 50 ml of water. To the solution is added a solution of 2.35 g of the crude tetramethylammonium phenylsulfate dissolved in 10 ml of water. The mixture is stirred for 7 hours 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 recrystallization from 1,2-dichloroethane, yielding 1.29 g of diphenyliodonium phenylsulfate as a white solid, mp. 129-132° C. The structure is confirmed by the 1H-NMR spectrum (CDCl6/DMSO-d6). δ [ppm]: 7.08 (t, 1H), 7.22-7.30 (m, 4H), 7.42 (t, 4H), 7.58 (t, 2H), 7.92 (d, 4H).

후처리

  1. extractionThe product is extracted with methylene chloride
  2. washthe organic layer is washed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue is purified by recrystallization from 1,2-dichloroethane

출처 및 근거

ORD 기록
ord-c0ed69020b804349b26ed13375f5a056
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06929896B2

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