HRID1196058

反应详情

EQUATION

反应方程式

HRID 1196058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1.62 g (24.9 mmol) of sodium azide in 10 ml of water is added to a solution of 6.3 g (16.6 mmol) of 2,2-dimethyl-6-fluoro-3-[2-(4-toluenesulfonyloxy)-ethyl]-chroman in 100 ml of ethanol. The mixture is boiled under reflux for 18 hours. After cooling, the ethanol is evaporated off in vacuo and water is added to the residue. The aqueous mixture is extracted with diethyl ether. The combined organic phases are washed with water, dried over sodium sulfate and concentrated by evaporation in vacuo, yielding 4.13 g (100% of the theoretical yield) of 3-(2-azidoethyl)-2,2-dimethyl-6-fluoro-chroman in the form of a light-yellow oil.

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling
  3. customthe ethanol is evaporated off in vacuo and water
  4. additionis added to the residue
  5. extractionThe aqueous mixture is extracted with diethyl ether
  6. washThe combined organic phases are washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated by evaporation in vacuo
  9. customyielding 4.13 g (100% of the