반응 #11728

ord-25061445411d408e8604d629580259c9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도at reflux overnight
  3. 3
    온도The reaction mixture was then cooled
  4. 4
    추출extracted with ethyl acetate
  5. 5
    건조The organic layer was dried over magnesium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated
  8. 8
    기타to give an orange oil

실험 절차

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (1.0 g, 3.35 mmol) in butanone (35 mL) was added 2-nitro-4-chlorophenol (0.64 g, 3.69 mmol), potassium carbonate (0.93 g, 6.7mmol) and potassium iodide (0.56 g, 3.35 mmol). The reaction mixture was heated at reflux overnight. The reaction mixture was then cooled, diluted with water and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, filtered and concentrated to give an orange oil. Chromatography on silica gel gave the title compound (1.35 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098212B2uspto-grants-2006_08