Reaktion #167030

ord-695b7d74410c487ca6e83285e3251756

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe organic layer was washed with water and brine
  2. 2
    Trocknendried over Na2SO4
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe obtained residue was purified by flash chromatography

Vorschrift

To a stirred solution of 2,7-dibromo-9H-fluorene (1.0 g, 3.1 mmol), KI (50 mg, 0.3 mmol) and KOH (750 mg, 13.3 mmol) in DMSO was added methyl iodide (0.42 mL, 6.8 mmol). The mixture was stirred at room temperature for 16 hours, then diluted with ethyl acetate (100 mL). The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was purified by flash chromatography to provide the desired product 2,7-Dibromo-9,9-dimethyl-9H-fluorene as a white solid (1.1 g, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841278B2uspto-grants-2014_09