Trifluoroacetic anhydride → Diphenyl-p-tolylsulfonium perfluorooctanesulfonate

HRID 1265964

反応式

HRID 1265964 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 30 minutes. After standing, the lower layer was concentrated and diluted with 340 parts of chloroform. The obtained chloroform solution was washed six times with 85 parts of ion-exchange water and concentrated to give 27.7 parts of 4-methylphenyldiphenylsulfonium perfluorooctanesulfonate, which is referred to herein as PAG3.

後処理

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

出典と根拠

ORDレコード
ord-e291b3deeda3401d959cef567596a5b2
出典データセット
uspto-grants-2003_04
特許番号
US06548221B2

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