反应详情

温度

0 °C

To a cooled (0° C.) solution of 1.5 g (4.27 mmol) of the product of Step C dissolved in 20 mL of acetonitrile, was added 2.12 g (6.4 mmol) of carbon tetrabromide, and 1.68 g (6.40 mmol) of triphenylphosphine. The reaction mixture was stirred 30 minutes at 0° C., then allowed to warm to room temperature and 0.5 mL (6.4 mmol) of acetone was added. The reaction mixture was stirred an additional 16 hours at room temperature, then filtered and evaporated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 5% ethyl acetate/hexane to afford 0.575 g (45%) of the title compound.

1. temperatureto warm to room temperature
2. stirringThe reaction mixture was stirred an additional 16 hours at room temperature
3. filtrationfiltered
4. customevaporated in vacuo
5. customThe residue was purified on a silica gel flash chromatography column
6. washeluted with 5% ethyl acetate/hexane