反应详情

温度

50 °C

(I1B): To a suspension of 3,5-dibromo-4-hydroxybenzonitrile (2.11 g, 7.62 mmol) in acetic acid (70 mL) was added sodium nitrite (2.63 g, 38.1 mmol) in small portion, evolving bubbles and bromine were observed. After addition, the mixture was stirred at 50° C. overnight. Reaction was cooled to room temperature; water (250 ml) was added and extracted with EtOAc for two times. The combined extracts were washed with water and brine, dried over MgSO4 filtered and the filtrate was concentrated to give yellow orange solid. The solid was treated with small amount of MeOH, collected by filtration, rinsed with MeOH, dried to afford 1.56 g of 3-bromo-4-hydroxy-5-nitrobenzonitrile as yellow solid.

1. additionAfter addition
2. customReaction
3. temperaturewas cooled to room temperature
4. extractionextracted with EtOAc for two times
5. washThe combined extracts were washed with water and brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationthe filtrate was concentrated
9. customto give yellow orange solid
10. filtrationcollected by filtration
11. washrinsed with MeOH
12. customdried