反应详情

To a solution of 1.00 g (2.985 mmol) of the product of Example 3 in 100 mL of CHCl3 was added 0.531 g (2.985 mmol) of N-bromosuccinimide and 0.025 g of AIBN. The resulting mixture was heated to reflux for 18 h and then an additional 0.411 g of NBS and 0.013 g of AIBN were added to the reaction. After refluxing the reaction for another 5 h the reaction mixture was cooled to room temperature, washed with sodium sulfite solution and water, dried over MgSO4, filtered and concentrated in vacuo. The residue was triturated with ether-hexanes to provide 0.62 g (50%) of the desired product as a white solid. EI Mass Spec 413 (M+).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 18 h
3. temperatureAfter refluxing
4. customthe reaction for another 5 h the reaction mixture
5. washwashed with sodium sulfite solution and water
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was triturated with ether-hexanes