反应详情

A solution of the product from Example 58, Part C (1.0 g, 4.74 mmol) and dibenzoyl peroxide (287 mg, 1.19 mmol) in chlorobenzene (24 mL) at reflux was treated in four portions with N-bromosuccinimide (843 mg, 4.74 mmol) over 30 min. The mixture was then stirred at reflux for 2 h. The mixture was cooled, filtered and concentrated and purified by column chromatography on silica gel, eluting with 7-30% chloroform in hexanes. The procedures afforded the title compound as a light yellow oil (438 mg, 32%).

1. temperatureat reflux for 2 h
2. temperatureThe mixture was cooled
3. filtrationfiltered
4. concentrationconcentrated
5. custompurified by column chromatography on silica gel
6. washeluting with 7-30% chloroform in hexanes