N-Methoxy-N-methylacetamide → 1-(3-Bromophenyl)propan-2-one

HRID 30356

反応式

HRID 30356 の反応式
CON(C)[C:4](=[O:6])[CH3:5].[Br:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[CH2:12][Mg]Br>CCOCC>[Br:8][C:9]1[CH:10]=[C:11]([CH2:12][C:4]([CH3:5])=[O:6])[CH:15]=[CH:16][CH:17]=1

参加物

4

反応条件

温度
0 °C

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).

後処理

  1. customthe reaction mixture was partitioned between hexane and saturated aqueous ammonium chloride
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-fc7cef611e73475ab104272aeb826061
出典データセット
uspto-grants-2008_09
特許番号
US07423067B2

関連ノート

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