反应详情

To a solution of diethyl 2-(2-(2-iodoethoxy)ethoxy)ethylphosphonate (1 eq) in EtOH (0.2 M) was added sodium azide (5 eq) in water (1.4 M). The reaction mixture was heated at reflux overnight. The mixture was then diluted with water, extracted with EtOAc (3 times). The combined organic layers were washed brine, dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5% MeOH/DCM to give diethyl 2-(2-(2-azidoethoxy)ethoxy)ethylphosphonate as colorless oil.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. extractionextracted with EtOAc (3 times)
4. washThe combined organic layers were washed brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated en vaccuo
7. customThe crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO)