HRID374342

反应详情

EQUATION

反应方程式

HRID 374342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperaturecooled
  2. custompartitioned between water (200 ml) and toluene (200 ml) and toluene (200 ml)
  3. customthe layers separated
  4. extractionThe aqueous layer was extracted with toluene (2×200 ml)
  5. dry with materialthe combined organic extracts dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure