반응 #65932

ord-8ffda47fa00c4b12a1a6271460898719

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution was refluxed for 1 hour
  2. 2
    추출extracted with toluene
  3. 3
    건조The organic phase was dried with sodium sulfate
  4. 4
    기타evaporated to dryness
  5. 5
    기타The residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420151uspto-grants-1995_05