反应详情

A solution of 4-[(biphenyl-4-carbonyl)amino]-2-methoxy benzoic acid (2.78 g; 8 mmol) in CHCl3 (175 mL) was cooled until it became cloudy (approx. 40° C.) and BBr3 (1.5 mL; 16 mmol) was added over 2 minutes. The mixture was allowed to warm slightly with stirring for 2 hours after which time another 1.5 mL BBr3 (16 mmol) was added and the reaction mixture was left to warm to room temperature overnight. The resulting slurry was added brine (50 mL) and the organic solvent was removed in vacuo. The resulting solid was Isolated by filtration, washed with H2O, air dried, refluxed in 99% EtOH (100 mL), cooled and filtered to yield 2.2 g (82%) of a white solid. Mp. 266° C. (decomposes).

1. additionwas added over 2 minutes
2. temperatureto warm slightly
3. additionwas added
4. waitthe reaction mixture was left
5. customthe organic solvent was removed in vacuo
6. customThe resulting solid was Isolated by filtration
7. washwashed with H2O, air
8. customdried
9. temperaturerefluxed in 99% EtOH (100 mL)
10. temperaturecooled
11. filtrationfiltered