HRID1750227

反应详情

EQUATION

反应方程式

HRID 1750227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 200 g cyclohexene and 30.7 g iodine in 800 ml of anhydrous dioxane was added 611.7 g of chloramine T. The mixture was stirred at 80° C. for 10 h. After cooling to room temperature the mixture was poured into ice water and extracted with ethyl acetate twice. The combined organic phases were dried over sodium sulphate and concentrated and the residue was purified by chromatography (Silica, hexane/Ethyl acetate) to afford 180 g (29%) of) 7-(Toluene-4-sulfonyl)-7-aza-bicyclo[4.1.0]heptane as a white solid.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the mixture
  2. extractionextracted with ethyl acetate twice
  3. dry with materialThe combined organic phases were dried over sodium sulphate
  4. concentrationconcentrated
  5. customthe residue was purified by chromatography (Silica, hexane/Ethyl acetate)