Toluene → HCID 22625512、化合物

HRID 277683

反応式

HRID 277683 の反応式
[I:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=O.[F:9][C:10]([F:21])([F:20])[CH:11]([F:19])[C:12]([F:18])([F:17])[S:13]([OH:16])(=[O:15])=[O:14].[C:22]1([CH3:28])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>ClCCl>[F:21][C:10]([F:9])([F:20])[CH:11]([F:19])[C:12]([F:17])([F:18])[S:13]([O-:16])(=[O:14])=[O:15].[CH3:28][C:22]1[CH:27]=[CH:26][C:25]([I+:1][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 1140TolueneHCID 92125IodosylbenzeneHCID 97946281-Propanesulfonic acid, 1,1,2,3,3,3-hexafluoro-

生成物 1

HCID 22625512HCID 22625512、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred suspension of 4.40 g (20 mmol) of iodosylbenzene in 100 ml of dichloromethane was added dropwise 4.64 g (20 mmol) of 3,3,3,2,1,1-hexafluoropropane sulfonic acid at 0° C. under exclusion of moisture. The mixture was stirred at room temperature for 2 hours. The temperature was returned to 0° C. again. 1.84 mg (20 mmol) of toluene was added dropwise. After the addition, stirring was continued at room temperature for additional 1 hour. The solvent was evaporated. The oily residue was dissolved in diethyl ether. After cooling, crystals of 4-methylphenyl phenyl iodonium 3,3,3,2,1,1-hexafluoropropane sulfonate were obtained. The crystals were washed with hexane.

後処理

  1. customwas returned to 0° C.
  2. additionAfter the addition
  3. stirringstirring
  4. waitwas continued at room temperature for additional 1 hour
  5. customThe solvent was evaporated
  6. dissolutionThe oily residue was dissolved in diethyl ether
  7. temperatureAfter cooling

出典と根拠

ORDレコード
ord-ddf0c014f98f40ba8f24c89467f58f9f
出典データセット
uspto-grants-2002_03
特許番号
US06358665B1

関連ノート

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