反应详情

To a solution of 1.70 g (5.86 mmol) of the product from Step A dissolved in 20 mL of CCl4 was added 1.04 g (5.86 mmol) of N-bromosuccinimide and 50 mg (catalytic amount) of AIBN. The reaction mixture was stirred and heated at reflux for 7 hours, then an additional 0.20 g of NBS was added. The reaction was refluxed for 48 hours, then cooled and concentrated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 10% ethyl acetate/hexane to afford 0.730 g (34%) of the title compound.

1. temperatureheated
2. temperatureat reflux for 7 hours
3. temperatureThe reaction was refluxed for 48 hours
4. temperaturecooled
5. concentrationconcentrated in vacuo
6. customThe residue was purified on a silica gel flash chromatography column
7. washeluted with 10% ethyl acetate/hexane