反应详情

To a stirred solution of concentrated nitric acid (6.8 mL, 101.0 mmol) in concentrated sulfuric acid (60 mL) was slowly added 3-bromo-4-fluorobenzaldehyde (10 g, 49.5 mmol) at 0° C. After the addition was completed, the ice bath was removed, and the reaction was allowed to warm to room temperature and stirred for 3 hours. The mixture was poured into ice water and extracted with ethyl acetate (200 mL). The organic layer was concentrated to give the title compound as a yellow solid (crude, 12 g, 100%), which was used directly for the next step without further purification.

1. customat 0° C
2. additionAfter the addition
3. customthe ice bath was removed
4. additionThe mixture was poured into ice water
5. extractionextracted with ethyl acetate (200 mL)
6. concentrationThe organic layer was concentrated