HRID1032439
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 18 hours
- temperatureAfter cooling
- customthe ethanol is evaporated off in vacuo and water
- additionis added to the residue
- extractionThe aqueous mixture is extracted with diethyl ether
- washThe combined organic phases are washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated by evaporation in vacuo
- customyielding 4.13 g (100% of the