反应详情

1.0 of 3,5-Dichloro-4-(1-methyl-2,2,3,3,3-pentafluoropropoxy)aniline was placed in a flask to which was added 15 mL of 1,2-dichloroethane. With stirring, 0.62 g 2.6-difluorobenzoyl isocyanate was added all at once to the mixture. The mixture was warmed to near reflux for one hour then cooled to room temperature and stirred overnight. It was then concentrated under vacuum to give 2.30 g crude product. The product was recrystallized from toluene, giving 208 mg of 1-(2,6-difluorobenzoyl)-3-[3,5-dichloro-4-(1-methyl-2,2,3,3,3-pentafluoropropoxy)phenyl]urea. 1H NMR: 10.59 (s, 1H) 9.58 (s, 1H), 7.34 (m, 3H), 7.07 (t, J=8.4 Hz,2H), 5.09 (m, 1H). MS: 506 m/z. IR:1746(s), 1710(s), 1539(s), 1470(m).

1. temperatureThe mixture was warmed
2. temperatureto near reflux for one hour
3. stirringstirred overnight
4. concentrationIt was then concentrated under vacuum
5. customto give 2.30 g crude product
6. customThe product was recrystallized from toluene