Reaktion #58634

ord-fc7cef611e73475ab104272aeb826061

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction mixture was partitioned between hexane and saturated aqueous ammonium chloride
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Waschenwashed with brine
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated to dryness

Vorschrift

To a solution of N-methoxy-N-methylacetamide (10 g, 0.10 mol) in 200 mL of ether at 0° C. was added 3-bromobenzylmagnesium bromide (0.25 M, 200 mL, 50 mmol). After stirring at 0° C. for 2 h, the reaction mixture was partitioned between hexane and saturated aqueous ammonium chloride. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness to give the title compound, which was used without further purification. 1H NMR (500 MHz, CD3OD): δ 7.5-7.1 (m, 4H), 3.78 (s, 2H), 2.19 (s, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423067B2uspto-grants-2008_09