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

HRID 1434495

反応式

HRID 1434495 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

In 10 ml of toluene was dissolved 2 g of thianthrene-S-oxide and the solution was cooled with ice. Then, 2.8 ml of trifluoroacetic anhydride and 1.2 ml of nonafluorobutanesulfonic acid were added thereto, followed by stirring for one hour. Diisopropyl ether was added thereto and the supernatant solution was removed. The residue was purified by a silica gel column (chloroform/methanol=19/1) to obtain 4.4 g of 5-(p-tolyl)thianthrenium nonafluorobutanesulfonate. 1H-NMR (400 MHz, CDCl3): σ 2.34 (s, 3H), 7.08 (d, 2H), 7.22 (d, 2H), 7.78 (m, 6H), 8.65 (d, 2H).

後処理

  1. temperaturethe solution was cooled with ice
  2. customthe supernatant solution was removed
  3. customThe residue was purified by a silica gel column (chloroform/methanol=19/1)

出典と根拠

ORDレコード
ord-fe3cbaa672e540b292fbcce13e566fe5
出典データセット
uspto-grants-2009_11
特許番号
US07615330B2

関連ノート

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