反应详情

温度

45 °C

13.2 g (0.060 mols) of (I) are dissolved at room temperature in 80 ml of CH2Cl2 under stirring, then 11.8 g (0.066 mols) of N-bromosuccinimide of purity above 98% and 0.70 g (0.003 mols) of di-tert-butyl-peroxalate are added under stirring. The reaction mixture is subjected to mild nitrogen stream for 5 minutes, then heated to 45° C. and stirred at this temperature for 85 minutes. The resulting suspension is added with 100 ml of demineralized water and 3 grams of polyethylene glycol with average molecular weight 400, then refluxed for 5 hours under strong stirring. After decanting at 30° C., the organic phase is separated, dried over 4 g of Na2SO4, filtered and the resulting solution is concentrated to 20 ml, added with 10 ml of hexane, cooled to 0-5° C. for 2 hours and filtered to obtain 8.64 g (61%) of (VI), m.p. 110-112° C.

1. stirringunder stirring
2. stirringstirred at this temperature for 85 minutes
3. temperaturerefluxed for 5 hours under strong stirring
4. customAfter decanting at 30° C.
5. customthe organic phase is separated
6. dry with materialdried over 4 g of Na2SO4
7. filtrationfiltered
8. concentrationthe resulting solution is concentrated to 20 ml
9. additionadded with 10 ml of hexane
10. temperaturecooled to 0-5° C. for 2 hours
11. filtrationfiltered