反応 #48403

ord-933edde9bb2146619a02fec26aa9054d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the mixture was extracted with ethyl acetate (3×)
  2. 2
    洗浄The combined organic extracts were washed with water (3×), saturated brine
  3. 3
    乾燥dried over sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated

実験手順

Sodium hydride (60% dispersion in mineral oil; 0.32 g, 8.03 mmol) was added to a solution of 6-phenylazepan-2-one (0.76 g, 4.02 mmol) in N,N-dimethylformamide (15 mL) at 0° C., followed by the addition of 2-bromoethyl methyl ether (0.837 g, 6.03 mmol), and the mixture was allowed to warm to ambient temperature. After 21 h, water was added and the mixture was extracted with ethyl acetate (3×). The combined organic extracts were washed with water (3×), saturated brine, dried over sodium sulfate, filtered and concentrated. MS 248 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745427B2uspto-grants-2010_06