反应详情

Add dropwise bromine (10.8 mL, 0.21 mol) in acetonitrile (260 mL) to a slurry of 6-hydroxy-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (51.8 g, 0.2 mol) in acetonitrile (400 mL) at 0° C. cooling with ice-water to keep the temperature between 2-5° C. Warm the reaction to ambient temperature and stir for 30 min. Pour the mixture into ice-cold water (2 L) to obtain a white precipitate. Collect the solid by vacuum filtration, wash with water and dry under vacuum at 105° C. Recrystallize the crude material in toluene/heptane and cool the mixture in an ice bath. Collect the solid by vacuum filtration, wash with heptane and dry under vacuum at 105° C. to obtain the desired intermediate as a white solid (54.63 g, 81%). MS (ES+) m/z: 338 (M+H)+.

1. custombetween 2-5° C
2. temperatureWarm
3. customthe reaction to ambient temperature
4. customto obtain a white precipitate
5. customCollect the solid
6. filtrationby vacuum filtration
7. washwash with water
8. customdry under vacuum at 105° C
9. customRecrystallize the crude material in toluene/heptane
10. temperaturecool the mixture in an ice bath
11. customCollect the solid
12. filtrationby vacuum filtration
13. washwash with heptane
14. customdry under vacuum at 105° C.