反応 #352175

ord-cd77eb6c5c3f422195b7d78a5c25f98e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution was refluxed for 1 hour
  2. 2
    抽出extracted with toluene
  3. 3
    乾燥The organic phase was dried with sodium sulfate
  4. 4
    その他evaporated to dryness
  5. 5
    その他The residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9

実験手順

3-Dipropylamino-5-aminochroman (Example 14; 0.60 g, 2.42 mmol) was dissolved in acetic acid (10 ml) and 2,5-dimethoxytetrahydrofuran (0.40 g, 3.0 mmol) was added. The solution was refluxed for 1 hour. The solution was neutralized with NaOH (aq.) and extracted with toluene. The organic phase was dried with sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9 to give the title compound. 13C-NMR: 111.75 21.89 24.81 52.69 53.15 67.94 108.93 115.67 118.22 118.44 121.87 127.22 141.47 155.27

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05646309uspto-grants-1997_07