Toluene → HCID 22625479、化合物

HRID 277693

反応式

HRID 277693 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:25])([F:24])[C:11]([F:23])([F:22])[C:12]([F:21])([F:20])[C:13]([F:19])([F:18])[S:14]([OH:17])(=[O:16])=[O:15].[C:26]1([CH3:32])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>ClCCl>[F:25][C:10]([F:9])([F:24])[C:11]([F:22])([F:23])[C:12]([F:20])([F:21])[C:13]([F:18])([F:19])[S:14]([O-:17])(=[O:16])=[O:15].[CH3:32][C:26]1[CH:31]=[CH:30][C:29]([I+:1][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[CH:28][CH:27]=1

参加物

5

反応物 3

HCID 1140TolueneHCID 67815Perfluorobutanesulfonic acidHCID 92125Iodosylbenzene

生成物 1

HCID 22625479HCID 22625479、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 6.0 g (20 mmol) of nonafluorobutane 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 g (20 mmol) of toluene was added dropwise. After the addition, stirring was continued at room temperature for additional 1 hour. The solvent as evaporated. The oily residue was dissolved in diethyl ether. The solution was cooled to obtain crystals of 4-methylphenyl phenyl iodonium nonafluorobutane sulfonate. The crystals were washed with hexane. The yield was 6.7 g.

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 as evaporated
  6. dissolutionThe oily residue was dissolved in diethyl ether
  7. temperatureThe solution was cooled

出典と根拠

ORDレコード
ord-cf4db4ad515e42cfba3f9d0f4ce22fea
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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