反应详情

To a solution of tert-butyl carbamate 155 (300 mg, 1.10 mmol) in THF (5 mL) at 0° C. is added sodium hydride (53 mg, 1.32 mmol, 60% dispersion in mineral oil) in one portion. After stirring 15 minutes, iodomethane is added (82 μL, 1.32 mmol) and the reaction mixture warmed to RT and stirred 16 h. The reaction is then quenched with 5% citric acid (10 mL) and extracted into EtOAc (2×10 mL). The combined organic phases are dried over Na2SO4 and purified by column chromatography (70% EtOAc in heptane) to give the title compound.

1. stirringstirred 16 h
2. customThe reaction is then quenched with 5% citric acid (10 mL)
3. extractionextracted into EtOAc (2×10 mL)
4. dry with materialThe combined organic phases are dried over Na2SO4
5. custompurified by column chromatography (70% EtOAc in heptane)