反应详情

To a solution of 8-azaspiro[4.5]dec-2-ene (2.74 g, 20 mmol) in Et3N (4.2 mL, 30 mmol) and DCM (100 mL) at 0° C. was added dropwise benzyl chloroformate (3.4 mL, 24 mmol). After 1 h, the solution was partitioned between H2O-DCM and the aqueous phase was extracted several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated and purified via column chromatography (silica, 10% EtOAc in hexanes) yielding the title compound (3.85 g, 71%) as a yellow oil: LCMS (ES) m/e 272 (M+H)+.

1. customthe solution was partitioned between H2O-DCM
2. extractionthe aqueous phase was extracted several times with DCM
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated
5. custompurified via column chromatography (silica, 10% EtOAc in hexanes)