反应详情

A solution of ethyl N-benzyloxycarbamate (7.80 g.) in absolute ethanol (5 ml.) was added dropwise to a solution of sodium ethoxide in absolute ethanol [Na: 920 mg., absolute C2H5OH: 100 ml.] at 70° C. and the mixture was stirred at the same temperature for 30 minutes. To the mixture was added dropwise dibutyl 3-chloropropylphosphonate (10.8 g.), whereafter the reaction mixture was refluxed with stirring for 22 hours. The resultant mixture was cooled to give precipitates, which were filtered off. The filtrate was concentrated under reduced pressure to give a residue. To the residue was added ethyl acetate (100 ml.) and water (50 ml.). The ethyl acetate layer was separated, dried over magnesium sulfate and then concentrated under reduced pressure to give an oily residue (16.6 g.). The residue was subjected to column chromatography on silica gel with an eluent (chloroform). Fractions containing the object compound were collected and concentrated under reduced pressure to give oily dibutyl 3 -(N-benzyloxy-N-ethoxycarbonylamino)propylphosphonate (7.33 g.)

1. temperaturewhereafter the reaction mixture was refluxed
2. stirringwith stirring for 22 hours
3. customto give
4. customprecipitates
5. filtrationwhich were filtered off
6. concentrationThe filtrate was concentrated under reduced pressure
7. customto give a residue
8. customThe ethyl acetate layer was separated
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure
11. customto give an oily residue (16.6 g.)
12. additionFractions containing the object compound
13. customwere collected
14. concentrationconcentrated under reduced pressure