反应详情

After dissolving tert-butyl N-(5-cyano-2-ethoxy-4-methylbenzoyl)-N-methylcarbamate (79.6 g) in carbon tetrachloride, azobisisobutyronitrile (4.1 g) was added and the mixture was heated to reflux. N-bromosuccinimide (50.3 g) was gradually added to the reaction mixture in small portions at a time. After heating to reflux for 2 hours, the mixture was filtered. The filtrate was concentrated and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (29.81 g) as a white solid.

1. additionwas added
2. temperaturethe mixture was heated to reflux
3. temperatureAfter heating
4. temperatureto reflux for 2 hours
5. filtrationthe mixture was filtered
6. concentrationThe filtrate was concentrated
7. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)