تفاعل #461524

ord-675d8aeb613b497fb27fbbfcd8dd66fc

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled
  2. 2
    أخرىpartitioned between water (200 ml) and toluene (200 ml) and toluene (200 ml)
  3. 3
    أخرىthe layers separated
  4. 4
    استخلاصThe aqueous layer was extracted with toluene (2×200 ml)
  5. 5
    تجفيفthe combined organic extracts dried over magnesium sulphate
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05166406uspto-grants-1992_11