反应详情

温度

80 °C

A mixture of di-tert-butyl (5-methylpyridin-2-yl)imidodicarbonate (Compound 309C, 5.66 g, 18.4 mmol), NBS (3.92 g, 22 mmol), and benzoyl peroxide (0.444 g, 1.84 mmol) in CCl4 (30 mL) was heated at 80° C. for 6 h. The mixture was cooled to room temperature, the solids were filtered off and the filtrate was concentrated. The residue was purified by silica gel chromatography (EtOAc/heptane: 1:1) to give 4.66 g of di-tert-butyl [5-(bromomethyl)pyridin-2-yl]imidodicarbonate (yield: 65%).

1. temperatureThe mixture was cooled to room temperature
2. filtrationthe solids were filtered off
3. concentrationthe filtrate was concentrated
4. customThe residue was purified by silica gel chromatography (EtOAc/heptane: 1:1)