Trifluoromethanesulfonic anhydride → HCID 59611359, Verbindung

HRID 417748Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 417748
[O:1]([S:9]([C:12]([F:15])([F:14])[F:13])(=[O:11])=[O:10])S(C(F)(F)F)(=O)=O.[Br:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[S:27][C:26]3[CH:28]=[C:29](O)[CH:30]=[CH:31][C:25]=3[CH:24]=2)=[CH:19][CH:18]=1>N1C=CC=CC=1>[Br:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[S:27][C:26]3[CH:28]=[C:29]([O:1][S:9]([C:12]([F:13])([F:14])[F:15])(=[O:10])=[O:11])[CH:30]=[CH:31][C:25]=3[CH:24]=2)=[CH:19][CH:18]=1

Komponenten

4

Versuchsvorschrift

Tf2O was added slowly to a mixture of 2-(4-bromo-phenyl)-benzo[b]thiophen-6-ol (200 mg, 0.66 mol) in pyridine (3 mL) at 0° C. with stirring. The mixture was stirred at ambient temperature for 16 hours before quenched with NaHCO3 solution. The mixture was extracted with ethyl acetate (50 mL). The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was used for next step reaction without further purification.

Aufarbeitung

  1. stirringThe mixture was stirred at ambient temperature for 16 hours
  2. custombefore quenched with NaHCO3 solution
  3. extractionThe mixture was extracted with ethyl acetate (50 mL)
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe obtained residue was used for next step reaction without further purification

Quellen und Nachweise

ORD-Eintrag
ord-ca9bc5dcdc234be59f3b2f5ce7c42491
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08088368B2

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