Trifluoroacetic anhydride → Diphenyl-p-tolylsulfonium perfluorooctanesulfonate

HRID 1699597

反応式

HRID 1699597 の反応式
[C:1]1([S:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.[F:28][C:29]([F:56])([S:52]([OH:55])(=[O:54])=[O:53])[C:30]([F:51])([F:50])[C:31]([F:49])([F:48])[C:32]([F:47])([F:46])[C:33]([F:45])([F:44])[C:34]([F:43])([F:42])[C:35]([F:41])([F:40])[C:36]([F:39])([F:38])[F:37]>C1(C)C=CC=CC=1>[F:56][C:29]([F:28])([S:52]([O-:55])(=[O:54])=[O:53])[C:30]([F:50])([F:51])[C:31]([F:49])([F:48])[C:32]([F:46])([F:47])[C:33]([F:45])([F:44])[C:34]([F:43])([F:42])[C:35]([F:41])([F:40])[C:36]([F:39])([F:38])[F:37].[CH3:36][C:35]1[CH:30]=[CH:31][C:32]([S+:7]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:33][CH:34]=1

参加物

5

反応物 3

HCID 9845Trifluoroacetic anhydrideHCID 13679Diphenyl sulfoxideHCID 74483Perfluorooctanesulfonic acid

生成物 1

HCID 21863659Diphenyl-p-tolylsulfonium perfluorooctanesulfonate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
2 °C

実験手順

Into a four-necked flask were charged 8.0 parts of diphenylsulfoxide and 80.0 parts of toluene, and the mixture was cooled to 2° C. Then, 16.6 parts of trifluoroacetic anhydride and 19.8 parts of perfluorooctanesulfonic acid were added and the mixture was stirred at the same temperature for 30minutes. After standing, the lower layer was concentrated and diluted with 340 parts of chloroform. The obtained chloroform solution was washed 6 times with 85 parts of ion-exchange water and concentrated to give 27.7 parts of 4-methylphenyldiphenylsulfonium perfluorooctanesulfonate.

後処理

  1. concentrationthe lower layer was concentrated
  2. additiondiluted with 340 parts of chloroform
  3. washThe obtained chloroform solution was washed 6 times with 85 parts of ion-exchange water
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-80458f4327504e61a3c9968496179399
出典データセット
uspto-grants-2002_02
特許番号
US06348297B1

関連ノート

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