Reaktion #1780320

ord-35f862ec1db543008e6a499e0857a2f9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigequenched with ice/water
  2. 2
    Extraktionextracted with methylene chloride
  3. 3
    WaschenThe organic phases were washed with water and aqueous sodium bicarbonate solution
  4. 4
    Sonstigedried
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe residue was chromatographed on silica gel

Vorschrift

To a solution of 5-fluoro-3-isobutyl-benzo[b]thiophene 0.55 g) in chloroform (10 ml) was added chlorosulfonic acid (1.54 g), and the resulting mixture was stirred at rt for 3 h, quenched with ice/water, and extracted with methylene chloride. The organic phases were washed with water and aqueous sodium bicarbonate solution, dried and concentrated. The residue was chromatographed on silica gel using heptane/ethyl acetate as eluent to obtain the title compound (0.49 g) as a colorless oil. MS (EI): 306.8 (M)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08158655B2uspto-grants-2012_04