反応 #58634

ord-fc7cef611e73475ab104272aeb826061

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the reaction mixture was partitioned between hexane and saturated aqueous ammonium chloride
  2. 2
    その他The organic layer was separated
  3. 3
    洗浄washed with brine
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    ろ過filtered
  6. 6
    濃縮concentrated to dryness

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07423067B2uspto-grants-2008_09