反応 #2069934

ord-5de4ecf04c544c78a0f7396164686f22

反応方程式

CC(C)OC(C)C
diisopropyl ether
O=C(OC(=O)C(F)(F)F)C(F)(F)F
trifluoroacetic anhydride
O=S(=O)(O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
nonafluorobutanesulfonic acid
O=S1c2ccccc2Sc2ccccc21
thianthrene-S-oxide
Cc1ccc([S+]2c3ccccc3Sc3ccccc32)cc1.O=S(=O)([O-])C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
5-(p-tolyl)thianthrenium nonafluorobutanesulfonate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度ice-cooled
  2. 2
    その他after removing the supernatant
  3. 3
    その他the residue was purified through a silica gel column (chloroform/methanol=19/1)

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. Subsequently, 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. 1H-NMR (400 MHz, CDCl3): δ 2.34 (s, 3H), 7.08 (d, 2H), 7.22 (d, 2H), 7.78 (m, 6H), 8.65 (d, 2H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07541131B2uspto-grants-2009_06