反应详情

温度

100 °C

To a solution of tert-butyl (1-(4-cyanophenyl)cyclopropyl)carbamate (D15) (1.5 g, 5.81 mmol) in dimethylformamide (15 ml), NH4Cl (530 mg, 9.90 mmol) was added under nitrogen atmosphere, followed by addition of sodium azide (650 mg, 9.9 mmol). The reaction mixture was heated to 100° C. overnight, then cooled to room temperature with ice-water bath. Water and ethylacetate (100 ml) was added. The organic layer was separated and the solvent was removed. The residue was purified by column chromatography eluting with a mixture petroleum ether/ethyl acetate (1:1). Collected fractions after solvent evaporation afforded the title compound (D16) (830 mg) as a yellow solid.

1. temperaturecooled to room temperature with ice-water bath
2. customThe organic layer was separated
3. customthe solvent was removed
4. customThe residue was purified by column chromatography
5. washeluting with a mixture petroleum ether/ethyl acetate (1:1)
6. customCollected fractions after solvent evaporation