HRID992381

反应详情

EQUATION

反应方程式

HRID 992381 的结构方程式

PROCEDURE

实验过程

A solution of 4.80 g (R)-5-acetoxy-1-chlorohexane (26.89 mmol) (prepared in accordance with procedures set forth in U.S. Pat. No. 5,629,423) was added to 5.39 g sodium iodide (36 mmol) in a round bottomed flask fitted with magnetic stirrer bar and a reflux condenser and refluxed for 12 h with stirring. Acetone was removed under reduced pressure. The crude product was partitioned between 60 ml ethyl acetate and 60 ml water layer. The organic layer was washed with 10% sodium thiosulphate solution followed by 20 ml water and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to yield 7 g (96%) (R)-5-Acetoxy-1-iodohexane.

WORKUP

后处理

  1. customfitted with magnetic stirrer bar and a reflux condenser
  2. temperaturerefluxed for 12 h
  3. customAcetone was removed under reduced pressure
  4. customThe crude product was partitioned between 60 ml ethyl acetate and 60 ml water layer
  5. washThe organic layer was washed with 10% sodium thiosulphate solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure