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

HRID 585029ノート

反応式

HRID 585029 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 22339003Diphenyliodonium phenylsulfate収率 35.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c0ed69020b804349b26ed13375f5a056
出典データセット
uspto-grants-2005_08
特許番号
US06929896B2

反応ノート

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