反应详情

温度

55 °C

To 1-benzylphosphorinane-l-oxide (5.39 g) were added nitric acid (1.94 ml) and sulfuric acid (15 ml) at 0° C., and the mixture was stirred at 50-60° C. for 2 hours. The reaction mixture was added to crushed ice-water, neutralized with ammonia solution and extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethanol/ethyl acetate=1:3→1:2) to give 1-(4-nitrobenzyl)phosphorinane-1-oxide (2.47 g)as pale yellow crystals.

1. additionThe reaction mixture was added
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated sodium chloride solution
4. dry with materialdried with magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was separated
7. custompurified with column chromatography (ethanol/ethyl acetate=1:3→1:2)