Reaktion #998507

ord-cc3fcbbff70244cc9db2baa5d51c899e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwash with brine
  2. 2
    Trocknendry the organic phase over anhydrous Na2SO4
  3. 3
    Sonstigeevaporate the solvent
  4. 4
    Sonstigepurify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1 and 4:1)

Vorschrift

Dissolve benzothiazol-6-yl-methanol (0.4 g, 2.55 mmol) in diethyl ether (10 mL) and add slowly a solution of phosphorus tribromide (0.7 g, 2.55 mmol) in diethyl ether (5 mL). Stir the reaction mixture for 2 h at ambient temperature, wash with brine, dry the organic phase over anhydrous Na2SO4, evaporate the solvent and purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1 and 4:1) to obtain the title compound as a white solid (0.5 g, 86%). MS (ES+) m/z: 229 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08022062B2uspto-grants-2011_09