반응 #461524

ord-675d8aeb613b497fb27fbbfcd8dd66fc

용매

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled
  2. 2
    기타partitioned between water (200 ml) and toluene (200 ml) and toluene (200 ml)
  3. 3
    기타the layers separated
  4. 4
    추출The aqueous layer was extracted with toluene (2×200 ml)
  5. 5
    건조the combined organic extracts dried over magnesium sulphate
  6. 6
    여과filtered
  7. 7
    농축concentrated under reduced pressure

실험 절차

To a solution of 2-acetylcyclohexanone (9.6 g, 0.068 mol), potassium carbonate (11.3 g, 0.082 mol) and benzyltriethylammonium chloride (0.3 g, 0.0013 mol) in toluene (26 ml), was added benzyl acrylate (16.72 g, 0.103 mol) at room temperature. The mixture was heated at 40° C. for 20 hours, cooled, partitioned between water (200 ml) and toluene (200 ml) and toluene (200 ml) and the layers separated. The aqueous layer was extracted with toluene (2×200 ml), the combined organic extracts dried over magnesium sulphate, filtered and concentrated under reduced pressure to provide the title compound as a pale yellow oil, (20.7 g), Rf. 0.2 (silica, hexane/diethyl ether, 2:1). The crude product was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05166406uspto-grants-1992_11