反応 #75953

ord-d5f1d0d3073d452b8ad7c8c476d8d731

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他resulting two-phase mixture
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    洗浄The combined organic extracts were washed with brine
  4. 4
    乾燥dried over anhydrous sodium sulfate
  5. 5
    その他evaporated

実験手順

A solution of sulfuryl chloride (12.4 mmol) in toluene (5 mL) was added dropwise via an additional funnel to a solution of ethyl isobutyrylacetate (12.4 mmol) in toluene (20 mL) over 5 minutes at room temperature. The resulting mixture was stirred at room temperature overnight. Water was added slowly and resulting two-phase mixture was basified with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, and evaporated to afford 2.2 g (84%) of product as a pale yellow oil: MH+=227.0, retention time (LC-MS)=2.77 min.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06699860B2uspto-grants-2004_03