反应详情

To a solution of diethyl 3-bromopropylphosphonate (1 eq) in EtOH (2 M) was added sodium azide (5 eq) in water (4 M). The reaction mixture was heated at reflux overnight. The mixture was then diluted with water, extracted with DCM three times. The combined organic layers are washed with brine, dried over anhydrous Na2SO4, and concentrated en vaccuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 80-100% EtOAc/Hex to give the product as a colorless oil.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. extractionextracted with DCM three times
4. washThe combined organic layers are washed with 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)