Diisopropyl Ether → 5-(p-Tolyl)thianthrenium nonafluorobutanesulfonate

HRID 2237343

反応式

HRID 2237343 の反応式
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6](=O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.[F:29][C:30]([F:45])([F:44])[C:31]([F:43])([F:42])[C:32]([F:41])([F:40])[C:33]([F:39])([F:38])[S:34]([OH:37])(=[O:36])=[O:35].C(O[CH:50]([CH3:52])[CH3:51])(C)C>C1(C)C=CC=CC=1>[F:45][C:30]([F:29])([F:44])[C:31]([F:42])([F:43])[C:32]([F:40])([F:41])[C:33]([F:38])([F:39])[S:34]([O-:37])(=[O:36])=[O:35].[C:50]1([CH3:51])[CH:52]=[CH:33][C:32]([S+:6]2[C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[S:13][C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]2=3)=[CH:31][CH:30]=1

参加物

6

反応物 4

HCID 7914Diisopropyl EtherHCID 9845Trifluoroacetic anhydrideHCID 67815Perfluorobutanesulfonic acidHCID 73220Thianthrene, 5-oxide

生成物 1

HCID 231378245-(p-Tolyl)thianthrenium nonafluorobutanesulfonate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Subsequently, 2 g of thianthrene-S-oxide was dissolved in 10 ml of toluene and ice-cooled, and 2.8 ml of trifluoroacetic anhydride and 1.2 ml of nonafluorobutanesulfonic acid were added thereto, followed by stirring for 1 hour. Furthermore, diisopropyl ether was added thereto and after removing the supernatant, the residue was purified through a silica gel column (chloroform/methanol=19/1) to obtain 4.4 g of 5-(p-tolyl)thianthrenium nonafluorobutanesulfonate.

後処理

  1. temperatureice-cooled
  2. customafter removing the supernatant
  3. customthe residue was purified through a silica gel column (chloroform/methanol=19/1)

出典と根拠

ORDレコード
ord-0bae235cd23141fa8e786f72bdaf2f18
出典データセット
uspto-grants-2010_05
特許番号
US07718344B2

関連ノート

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