反应详情

温度

30 °C

A solution of carbonic acid chloromethyl ester 2,6-dibromo-4-cyanophenyl ester (10.0 g, 27.1 mmol) in 30 mL of acetone was added sodium iodide (8.12 g, 54.1 mmol) and heated to 30° C. for 3 h. The acetone was removed, and the resulting slurry was treated with ether. The resulting white precipitated solids were filtered off, and the filtrate was then concentrated to afford tannish solids which was recrystallized from ether/hexanes to afford white solids (20 g, 96%). 1H-NMR (300 MHz, CDCl3) δ (ppm): 6.09 (s, 2H), 7.90 (s, 2H). Mp=103-105° C.

1. customThe acetone was removed
2. additionthe resulting slurry was treated with ether
3. customThe resulting white precipitated solids
4. filtrationwere filtered off
5. concentrationthe filtrate was then concentrated
6. customto afford tannish solids which
7. customwas recrystallized from ether/hexanes