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

HRID 1434495

반응식

HRID 1434495 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 231378245-(p-Tolyl)thianthrenium nonafluorobutanesulfonate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-fe3cbaa672e540b292fbcce13e566fe5
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615330B2

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