反应详情

温度

15 °C

Bromine (13.4 mL, 0.262 mol) was added dropwise over a period of 30 min to a cooled (ice bath) and stirred suspension of 2 (37.86 g, 0.131 mol) in water:t-BuOH=1:1 (1500 mL). Cooling bath was removed and the mixture was stirred at r.t. overnight. Then the solution was cooled to 15° C. and saturated aqueous solution of NaHCO3 (278 mL) was added. A yellow suspension, which was formed, was concentrated in vacuum (bath temperature <32° C.) until about 1000 mL of condensate was collected. The solid was filtered off, washed with water (200 mL), and dried in vacuum to afford 3 (40.85 g, 85%) as tan powder.

1. temperaturea cooled (ice bath)
2. temperatureCooling bath
3. customwas removed
4. stirringthe mixture was stirred at r.t. overnight
5. additionsaturated aqueous solution of NaHCO3 (278 mL) was added
6. customA yellow suspension, which was formed
7. concentrationwas concentrated in vacuum (bath temperature <32° C.) until about 1000 mL of condensate
8. customwas collected
9. filtrationThe solid was filtered off
10. washwashed with water (200 mL)
11. customdried in vacuum