反应详情

To a solution of benzyl 3,7-diazabicyclo[4.1.0]heptane-3-carboxylate (1.0 equiv.) in DCM (0.26M) was added diethyl phosphorochloridate (1.3 equiv.) and triethyl amine (1.5 equiv.). The reaction was stirred for 24 h, then concentrated to dryness. Added water and ethyl acetate, the organics were extracted, dried with Na2SO4, and concentrated. The crude was purified via silica gel column chromatography eluting with ethyl acetate and hexanes (50% to 100% ethyl acetate) to yield benzyl 7-(diethoxyphosphoryl)-3,7-diazabicyclo[4.1.0]heptane-3-carboxylate as a clear oil in 21% yield. LCMS (m/z): 369.0 (MH+).

1. concentrationconcentrated to dryness
2. extractionAdded water and ethyl acetate, the organics were extracted
3. dry with materialdried with Na2SO4
4. concentrationconcentrated
5. customThe crude was purified via silica gel column chromatography
6. washeluting with ethyl acetate and hexanes (50% to 100% ethyl acetate)