HRID1826472

反应详情

EQUATION

反应方程式

HRID 1826472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-cyclohexyloxyethyl 4-bromobenzenesulfonate (Preparation 86, 120 mg, 0.3 mmol) in acetone (5 ml) was added sodium iodide (90 mg, 0.6 mmol) and the reaction mixture was left to stir at room temperature for 18 h. A further equivalent of sodium iodide was added and the reaction mixture was stirred at room temperature for a further 18 h after which time the reaction mixture was heated to 80° C. for 5 h. The resulting precipitate was filtered and the filtrate was diluted with water (100 ml) and extracted with dichloromethane (100 ml). The extract was washed with brine (100 ml), dried (MgSO4) and concentrated in vacuo to give the title compound as a colourless oil (50 mg, 60%).

WORKUP

后处理

  1. waitthe reaction mixture was left
  2. stirringthe reaction mixture was stirred at room temperature for a further 18 h after which time the reaction mixture
  3. temperaturewas heated to 80° C. for 5 h
  4. filtrationThe resulting precipitate was filtered
  5. additionthe filtrate was diluted with water (100 ml)
  6. extractionextracted with dichloromethane (100 ml)
  7. washThe extract was washed with brine (100 ml)
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated in vacuo