反应详情

2-Amino-4-chlorobenzoic acid (0.3 g), 2-fluorophenylisocyanate (0.2 ml) and triethylamine (0.24 ml) were stirred in toluene (20 ml) for a week. More 2-fluorophenylisocyanate (0.1 ml) was added and stirring continued for another week. The mixture was concentrated to almost dry, water was added and the pH was adjusted to 1 with diluted HCl. Water was decanted and the residue was dissolved in warm 96% EtOH. The pH was adjusted to 1 again with 4N HCl resulting in the precipitation of a solid, which was filtered and dried to give 4-chloro-2-[3-(2-fluoro-phenyl)-ureido]-benzoic acid (0.25 mg). Mp.=195-197° C. 4-Chloro-2-[3-(3-trifluromethyl-phenyl)-ureido]-benzenesulfonamide (Compound 10):

1. waitcontinued for another week
2. concentrationThe mixture was concentrated
3. customto almost dry
4. additionwater was added
5. customWater was decanted
6. dissolutionthe residue was dissolved in warm 96% EtOH
7. customThe pH was adjusted to 1 again with 4N HCl resulting in the precipitation of a solid, which
8. filtrationwas filtered
9. customdried